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Freeze Drying - Fisher UK Extranet

1. PART DESCRIPTION 7726500 6 Port Manifold for use with Stoppering Tray Dryer Mounts between the Stoppering Tray Dryer and the base unit and provides 6 freeze dry valves 7537800 Cable Connect the RS232 output from the Freeze Dryer or Freeze Dryer Tray Dryer combination to an IBM compatible computer with a 9 pin serial data port 7537801 Cable Connects the RS232 output from the Freeze Dryer or Freeze Dryer Tray Dryer combination to an IBM compatible computer with a 25 pin serial data port 7761500 Isolation Valve Mounts between the Stoppering Tray Dryer and the base unit which provides a way to isolate the base unit vacuum system from the Stoppering Tray Dryer vacuum system 7756100 Tray with Slide Out Bottom 14 wide x 12 deep Stainless steel tray has separate bottom which slides out allowing serum bottles and ampules direct contact with the shelf to facilitate the drying process 7756200 Bulk Tray 15 wide x 11 1 2 deep Stainless steel tray will contain liquids for bulk drying 7756300 Shelf Spacers 2 1 2 high x 9 wide x 13 deep Two stainless steel spacers placed on one or two empty shelves assist stoppering of partial loads of small vials or bottles 7516200 Support Grid 7 wide x 7 deep Stainless steel tray with removable plastic grid provides support for stoppering ampules and other small specimen containers while stoppering under vacuum Grid holds 144 ampules of 12 mm diameter 60 Pr
2. Chapter 3 Getting Started E Solvent Safety Precautions Solvents used in the Stoppering Tray Dryer may be flammable or hazardous to your health Use extreme caution and keep sources of ignition away from the solvents When using flammable or hazardous solvents the vacuum pump must be vented to a fume hood Hazardous materials such as strong acids or bases radioactive substances and volatile organics must be handled carefully and promptly cleaned up if spilled If a sample is spilled in the collector chamber it must immediately be cleaned up WARNING The disposal of substances used in connection with this equipment may be governed by various Federal State or local regulations All users of this equipment are urged to become familiar with any regulations that apply in the user s area concerning the dumping of waste materials in or upon water land or air and to comply with such regulations Product Service Domestic 1 800 522 7658 International 816 333 8811 15 CHAPTER 4 Using Your STOPPERING TRAY DRYER After your Stoppering Tray Dryer has been installed as detailed in Chapter 3 Getting Started you are ready to begin using your Stoppering Tray Dryer Read this chapter to learn how to e operate the controls e understand the display e connect samples Do not use the Stoppering Tray Dryer in a manner not specified by the manufacturer refer to Appendix C Stoppering Tray Dryer Specifications Th
3. 3 deteriorate and require replacement The effective life of rubber parts depends upon both their usage and the surrounding environment Check all rubber hoses and gaskets and replace any that show signs of hardening permanent set or deterioration Using a soft cloth sponge or chamois and a mild non abrasive soap or detergent clean the acrylic chamber lid Using a soft cloth sponge or chamois and a mild non abrasive soap or detergent clean the exterior surfaces of the Freeze Dryer Liquid spray cleaners and polishes may be used on the exterior surfaces Do not use solvents to remove stains from the exterior surfaces as they may damage the finish Annually 1 Every 12 months or more often if the Freeze Dryer is operated in a dusty environment the refrigeration system condenser should be cleaned Using a vacuum cleaner with brush attachment clean the condenser to ensure proper airflow for peak performance Product Service Domestic 1 800 522 7658 International 816 333 8811 CHAPTER 6 Usinc THe RS232 RECEPTACLE The operation of the Freeze Dryer can be monitored using a computer when it is connected to the RS232 receptacle on the rear panel The computer cannot control the operation of the Freeze Dryer The monitored parameters are the collector temperature in C and vacuum in microbars When a Labconco Stoppering Tray Dryer is connected to a Labconco Freeze Dryer as detailed in the Stoppering Tray Dryer User s
4. 4 The Connect To dialogue box will open Using the down arrow selection button select the communication port to which the cable has been connected Press OK 5 The Com X Properties dialogue box will open Enter the appropriate data properties and press OK Product Service Domestic 1 800 522 7658 International 816 333 8811 37 Chapter 6 Using the RS232 Receptacle 6 When the Freeze Dryer main power switch is on the data will be transmitted and updated at the time intervals selected by the 38 user cone day 0 05 26 ERAM INDIO Hyper terminal 1 Fle EM view Cal Trade tado lurizo 2403 eme Piani fears jum iarna rerreto Product Service Domestic 1 800 522 7658 International 816 333 8811 B lt T 80V 16 SF 999C 999PG 9 gt TD lt PR 1S IRTR 18ST 26P1 25P2 999P3 9994 Bcl SUV 16 SI 999 999PG 9 UCPR LS IRIR 10S 26P1 25P2 999P3 999N 30 gt R lt T 8AV 14 SF 9990 999PG 92 TN lt PR 1S 1RTR 1AST 26P1 25P2 999P5 999 A gt B lt T 80V L amp 4 SF 9990 999PG 9 gt TD lt PR 1S IRTR 1 ST 26P1 25P2 999P3 999V 30 gt B lt T 20V 14 SF 999C 999PG 9 gt TD lt PR 15 IRTR 18ST 26P1 25P2 999P3 9994 30 gt Bel SUV 14 I 999 999P0 9 DePR 1S IRIR 18S 26P1 25P2 999P3 D99N 385 Bcl SUV 14 SI 999C 999PG 9 UC R LS IRIR 188 1 26D1 25P2 999P3 999N 39 R lt T 8AV 14 SF 9990 999PG 92TN lt PR 1S IRTR 1A8T 26P 1 26P2 999P9 9
5. 6L 7750601 Compressor 230V 50 Hz 6L 7750600 Compressor 230V 60 Hz 6L Cascade 7591800 Compressor 115V 60 Hz Hi Stage 6L Cascade 7591800 Compressor 115V 60 Hz Lo Stage 6L Cascade 7591801 Compressor 230V 50 Hz Hi Stage 6L Cascade 7591801 Compressor 230V 50 Hz Lo Stage 6L Cascade 7591802 Compressor 230V 60 Hz Hi Stage 6L Cascade 7591802 Compressor 230V 60 Hz Lo Stage DL 7592001 Compressor 230V 50 Hz DL 7592000 Compressor 230V 60 Hz 12L Cascade 7750601 Compressor 230V 50 Hz Hi Stage 12L Cascade 7750601 Compressor 230V 50 Hz Lo Stage 12L Cascade 7750600 Compressor 230V 60 Hz Hi Stage 12L Cascade 7750600 Compressor 230V 60 Hz Lo Stage 18L 7391801 Compressor 230V 50 Hz 18L 7391800 Compressor 239V 60 Hz 6 6L 7591800 Compressor 115V 60 Hz Shell Freezer 6L 7591801 Compressor 230V 50 Hz Shell Freezer 6L 7591802 Compressor 230V 60 Hz Shell Freezer 7 6L 7953800 Motor Fan 115V All 7953801 Motor Fan 230V 8 All 1302300 Switch 9 All 7403500 Label Control Panel All 7403501 Label Control Panel with Purge All 7403502 Label Control Panel with Purge and Shell Freezer Drying Chamber 10 All 7445500 Printed Circuit Board Control 11 All 7448000 Printed Circuit Board RS232 12 All 7728000 Drain Plug 13 All 1643600 O Ring 14 All 7645904 Drain Hose 15 All 7646000 Vacuum Hose Not Shown 16 6L 1336400 Power Cord 115V All 1342100 Power Cord 230V 17 All 7445400 Vacuum Sensor
6. Central Standard Time Visit Labconco s web site at http www labconco com or email Labconco at labconco labconco com Part 7403400 Rev C ECO C639 TABLE Or CONTENTS CHAPTER 1 INTRODUCTION Freeze Dry Process Freeze Dry Rates Freeze Dry Capacity Samples Containing Volatile Substances About This Manual Typographical Conventions CHAPTER 2 PREREQUISITES Electrical Requirements Location Requirements Vacuum Pump Requirements Chamber or Manifold Requirements CHAPTER 3 GETTING STARTED Unpacking Your Freeze Dryer Freeze Dryer Components Setting Up Your Freeze Dryer Vacuum Pump Connection Electrical Connection Drying Chamber or Drying Manifold Installation Chemical Resistance of Freeze Dryer Components Solvent Safety Precautions CHAPTER 4 USING YOUR FREEZE DRYER Freeze Dryer Controls Operation Checklist Vacuum Pump Ballast Setting Purge Valve Operating the Freeze Dryer Set Up Baffle Automatic Start Up Automatic Start Up with Purge Valve Manual Start Up Manual Start Up with Purge Valve DA EO ma oO o N N 10 12 13 14 14 14 16 18 19 21 21 21 22 22 25 25 25 26 26 Setting the Operating Vacuum Level Pre Freezing Samples Adding Sample Shut Down Defrosting Operating the Shell Freezer Operating the Vacuum Drying Chamber Alarms Power Failure Line Voltage Out of Range Temperature Out of Range Service Vacuum Pump Moisture in Collector CHAPTER 5 MAINTAINING YOUR FREEZE DRYE
7. 18 All 7515300 Temperature Sensor Collector Not Shown 19 6L 7515300 Temperature Sensor Shell Freezer Not Shown Product Service Domestic 1 800 522 7658 International 816 333 8811 55 Appendix A Freeze Dryer Components Item Model Part No Description 20 All 7515300 Temperature Sensor Drying Chamber Not Shown 21 6L 12L 18L 7404900 Wire Harness Not Shown 6L 12L Cascade 7446500 Wire Harness Not Shown 22 All 7514900 Wire Harness Control Not Shown 23 All 7418300 Wire Harness RS232 Not Shown 24 All 7432700 Valve Vacuum Bleed 25 6L 1363102 Valve Purge 115V All 1363103 Valve Purge 230V 26 All 7814600 Valve Drying Chamber 27 6L 7407300 Heater Drying Chamber 115V All 7407301 Heater Drying Chamber 230V 28 All 7429700 Moisture Sensor 29 6L 1289200 Relay Vacuum Pump 115V All 1289100 Relay Vacuum Pump 230V 30 All 1289200 Relay Refrigeration 31 All 7403800 Filter Vacuum Bleed Valve Product Service Domestic 1 800 522 7658 International 816 333 8811 Appendix A Freeze Dryer Components o Product Service Domestic 1 800 522 7658 International 816 333 8811 57 58 Appendix A Freeze Dryer Components Product Service Domestic 1 800 522 7658 International 816 333 8811 AprENDIX B FREEZE DRYER DIMENSIONS 2800 Tid INCHES CENTIMETERS Product Service Dome
8. 7542800 7542900 7543000 7543200 Flask Top 7544000 7544000 75442 00 7544200 7544200 7544400 7544400 7544400 7544400 Flask Top Adapter Diameter 1 2 1 2 3 4 3 4 3 4 3 4 3 4 3 4 3 4 Dimensions Flask Bottom HxD 76 mm x 34 mm 115 mm x 34 mm 68 mm x 59 2 mm 85 mm x 59 2 mm 145 mm x 59 2 mm 135 mm x 90 2 mm 190 mm x 90 2 mm 240 mm x 90 2 mm 380 mm x 90 2 mm Valves on the freeze dry systems drying chambers and manifolds offered in this catalog fit adapters of both 1 2 and 3 4 sizes Size information is provided for selecting adapters for older Labconco mod els and other freeze dryers Variety of adapters available You may select from glass or stainless steel adapters available straight or with 45 bend Required order separately Top seals easily The flexible silicone rubber top snaps on and off easily yet provides a reliable high vacuum seal o Only two pieces per flask The complete Fast Freeze Flask has only two components e a high strength borosilicate glass bottom to withstand extreme temperatures and high vacuum e a flexible non contaminating silicone rubber top No vacuum grease is necessary No threads hooks or springs are needed Entire flask may be autoclaved Adapters Add the Adapters for connecting the Fast Freeze Flasks to the valve ports on your drying chamber or manifold Choose borosilicate glass o
9. Domestic 1 800 522 7658 International 816 333 8811 15 Chapter 3 Getting Started Rubber and plastic components that have been exposed to damaging compounds should be removed and flushed with water The oil in the vacuum pump should be checked often It must be changed if it is cloudy shows particles or is discolored The useful life of vacuum pump oil can be extended if the vacuum pump is operated for an extended period of time after a freeze dry run This allows contaminants to be purged from the hot oil This must be done with the inlet to the pump blocked off to prevent air from free flowing through the pump This is accomplished by closing all sample valves on a clean dry freeze dry system and turning on the vacuum pump If the pump is operated at an elevated vacuum level gt 10mBar oil may be expelled from the pump and damage could occur Another way to extend the life of the vacuum pump is to install an optional secondary trap in the line between the Freeze Dryer and the vacuum pump Contact Labconco for ordering information With prudent maintenance the FreeZone Freeze Dry System will provide years of service Warranty on the affected parts will be voided if maintenance has been obviously neglected If you have questions about using specific compounds in the Freeze Dryer contact Labconco Technical Service at 1 800 821 5525 or 816 333 8811 or e mail labconco labconco com E Solvent Safety Precautions Solven
10. Domestic 1 800 522 7658 International 816 333 8811 Chapter 4 Using Your Freeze Dryer 7 Ifthe Shell Freezer is to be used for cold bath operation additional solvent may be added to submerge small flasks Do not fill pan more than 2 inches below the top of the stainless steel pan with vessels submerged Allow additional time for larger volumes of solvent to pull down in temperature 8 Always drain flammable solvents from the bath when the shell freezer is not in use and store the solvent in a suitable container This is accomplished by first pulling the drain hose out of the front panel of the unit and then removing the drain plug Place the hose in a suitable container to collect the solvent Operating the Vacuum Drying Chamber The built in drying chamber is designed for freeze drying small samples either in bulk or in small containers such as vials or 96 well plates It may be used in conjunction with other drying accessories that are mounted on top of the Freeze Dryer or independently If a manifold or chamber is mounted to the Freeze Dryer and is not in use close all of its valves If no drying accessory is installed on the Freeze Dryer place the supplied stopper in the center of the 3 0 accessory port that is on the top of the Freeze Dryer to seal the vacuum system Follow the steps below to operate the built in drying chamber 1 Start the Freeze Dryer Position the Vacuum Chamber valve on the top of the Freeze Dryer to the VEN
11. The first time Hyper Terminal is opened a dialogue box requesting an area code and phone number will appear Enter the appropriate numbers and continue 3 The Connection Description dialogue box will open Type in a user defined name and select an icon for the new connection Press OK 4 The Connect To dialogue box will open Using the down arrow selection button select the communication port to which the cable has been connected Press OK Product Service Domestic 1 800 522 7658 International 816 333 8811 39 Chapter 6 Using the RS232 Receptacle 5 The Com X Properties dialogue box will open Enter the appropriate data properties and press OK 40 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 6 Using the RS232 Receptacle 6 When the Freeze Dryer main power switch is on the data will be transmitted and updated at the time intervals selected by the user Product Service Domestic 1 800 522 7658 International 816 333 8811 41 CHAPTER 7 TROUBLESHOOTING Refer to the following if your Freeze Dryer fails to operate properly If the suggested corrective actions do not solve your problem contact Labconco for additional assistance Labconco Freeze Dry Systems that are clean dry and without samples attached should reach a vacuum of 0 133 mBar within 10 minutes and should achieve an ultimate vacuum of 0 033 mBar with
12. To release the vacuum move the Vacuum Release control to the OPEN position and shut off the vacuum pump using the switch on the base unit Air enters the vacuum chamber through the Back Fill port When the sound of air through the Back Fill port is no longer audible the chamber door is ready to open To backfill the chamber with a gas connect a cylinder of the desired gas to the Back Fill port The port will accept 1 8 tubing The bottle must be equipped with a regulator set to 15 psi maximum The gas can be metered with the Vacuum Release control and chamber pressure monitored with the freeze dry system s vacuum gauge Allow the vacuum pump to run for a few minutes while the gas enters to permit the back fill gas to surround the freeze dried sample When the vacuum pump is turned off air will enter the system through the vacuum break valve located between the vacuum pump and the collector chamber Product Service Domestic 1 800 522 7658 International 816 333 8811 29 Chapter 4 Using Your Stoppering Tray Dryer Alarms A number of unusual events may occur during a lyophilization procedure that can adversely effect the operation of the Stoppering Tray Dryer If an event occurs the alarm indicator will flash and the beeper will sound The beeper will automatically mute itself after one minute The specific alarm can be identified observing the display The following out of specification conditions will initiate an al
13. shipping however under certain circumstances it may be necessary to adjust the calibration of the temperature and or vacuum display or to modify alarm points Adjustments may be necessary if the Freeze Dryer requires service or if it is operating on a line voltage outside the voltage range at which the alarm was preset This DOES NOT mean that the Freeze Dryer may be operated at a voltage outside the ranges shown in Appendix C Temperature and Vacuum Display An offset may be added to the collector temperature or vacuum display Use an accurate traceable reference to compare the readings Temperature offset may be varied 5 C in 1 C increments Vacuum offset may be varied 0 020 mBar in 0 001 mBar increments Line Voltage Alarm Points The Freeze Dryer is designed to alarm if the line voltage varies more than 10 from nominal line voltage Models rated to operate on 115V are preset to alarm if the voltage drops below approximately 103V or rises above approximately 127V Models rated to operate on 230V will alarm if the voltage drops below Product Service Domestic 1 800 522 7658 International 816 333 8811 49 Chapter 8 Modifying Your Freeze Dryer Display approximately 206V or rises above approximately 254V Some models are designed to operate below these ranges see Appendix C In these cases it is permissible to lower the low voltage alarm point to prevent nuisance alarms from occurring Low line limit may be lowered in 5
14. switch to start the system When the system temperature stabilizes add or remove fluid from the reservoir to the level indicated by the label Apply vacuum to the unit and when the system is 0 133 mBar or less install the cap on the tank Remove the tubing Replace the caps on the valve and replace insulation and covers Heat Transfer Fluid Precautions The fluid s name and manufacturer are Name Lexol 542 Manufacturer Santa Barbara Chemical Co 927 Indio Muerto Santa Barbara CA 93140 805 963 7793 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 7 Troubleshooting WARNING The fluid used for heat transfer in this system is combustible and hazardous Leaks and spills should be attended to immediately Handling and Storage Precautions Dirty Solvent Store in accordance with all applicable regulations Tighten caps and store in a cool area Precautions if Material is Released or Spilled Spills should be contained immediately Spills may be soaked up with absorbent materials placed in closed containers labeled stored and disposed of properly Persons performing this work should wear adequate personal protective equipment and clothing Disposal of Non Recyclable Solvents Dispose of in accordance with all federal state and local health and pollution regulations Follow same guidelines as used when disposing kerosene Heat Transfer Fluid First Aid Procedures
15. to 40 C Maximum relative humidity 80 for temperatures up to 88 F 31 C decreasing linearly to 50 relative humidity at 104 F 40 C e Main supply voltage fluctuations not to exceed 10 of the nominal voltage e Transient over voltages according to Installation Categories II Over voltage Categories per IEC 1010 Temporary voltage spikes on the AC input line that may be as high as 1500V for 115V models and 2500V for 230V models are allowed e Used in an environment of Pollution degrees 2 i e where normally only non conductive atmospheres are present Occasionally however a temporary conductivity caused by condensation must be expected in accordance with IEC 664 Product Service Domestic 1 800 522 7658 International 816 333 8811 63 Appendix C Freeze Dryer Specifications 64 Wiring Diagram Catalog 77530xx and 77535xx 79340xx 115V 60 Hz Models DAT E LIES COMBGLE FREEZE Inv BO HE OV SoH LABCONCO PYM THOSS00 REYS WIRING DIAGRAM Product Service Domestic 1 800 522 7658 International 816 333 8811 Appendix C Freeze Dryer Specifications Wiring Diagram Catalog 79340xx 230V 50 or 60 Hz Models E f EST p Ci Si io TAg is E is aurreren E a h See ARE EE i LI Had E E Ucla oS O gEsa ij ae F pus E M za T EHRT i E JEENA m ECL PRODUCT GPTIGAS FTTFLEA ey A tal Product Service Domestic 1 800
16. vacuum pump is running depending on ambient temperature and humidity Cascade Freeze Dry Systems will achieve 84 C within 40 minutes Cascade Systems those that operate 84 consist of two vapor compression refrigeration systems in series connected together via a heat exchanger Each system has a compressor condenser capillary tube metering device and an evaporator During operation the evaporator of the high stage system refrigerates the condenser of the low stage system This takes place in the heat exchanger The low stage and high stage systems are balanced by design however sometimes that balance can be disrupted during operation and the unit will not function properly If the unit is overloaded or if the unit is defrosted and restarted in a short time interval system unbalance is possible If system unbalance occurs turn the Freeze Dryer off and allow the unit to soak at ambient temperature for 2 to 4 hours If any repairs are required on the refrigeration module contact your local laboratory supply dealer If your laboratory supply dealer is unable to provide assistance please call Labconco Repairs should only be undertaken by a competent refrigeration technician or through an authorized Labconco service agency 48 Product Service Domestic 1 800 522 7658 International 816 333 8811 CHAPTER 8 MopiFryinc Your FREEZE DRYER DisPLAY Your Freeze Dryer has been carefully calibrated and tested before
17. with the information following an exclamation icon may result in injury to the user or permanent damage to your Freeze Dryer e Important information is presented in capitalized type in IS paragraphs that are preceded by the pointer icon It is imperative that the information contained in these paragraphs be thoroughly read and understood by the user 6 Product Service Domestic 1 800 522 7658 International 816 333 8811 CHAPTER 2 PREREQUISITES Before you install your Freeze Dryer you need to prepare your site for installation Carefully examine the location where you intend to install your Freeze Dryer You must be certain that the area is level and of solid construction An electrical source must be located near the installation site Carefully read this chapter to learn e the electrical supply requirements e the vacuum pump requirements Refer to Appendix C Freeze Dryer Specifications for complete Freeze Dryer electrical and environmental conditions specifications and requirements Electrical Requirements The Freeze Dryer requires a dedicated electrical outlet This outlet requires a 20 Amp circuit breaker or fuse for models rated at 115V 60 Hz An outlet equipped with a 15 Amp circuit breaker or fuse is required for models rated at 230V 50 60 Hz The power cord on 115V models is equipped with a 20 Amp NEMA 5 20P plug The power cord on 230V models is equipped with a NEMA 6 20P plug If this does not match with t
18. 115V Or 1336600 1 Power Cord 230V 1880712 4 Screw 14 20 x 75 1905621 4 Nut 4 20 1911416 8 Washer 1 4 7353403 1 Cable RS 232 If you did not receive one or more of the components listed for your Stoppering Tray Dryer or if any of the components are damaged contact Labconco Corporation immediately for further instructions 10 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 3 Getting Started Setting Up Your Stoppering Tray Dryer After you verify receipt of the proper components move your Stoppering Tray Dryer to the location where you want to install it Then follow the steps listed below Installing the Tray Dryer on the Freeze Dry System The following tools are required to install the Stoppering Tray Dryer onto a FreeZone Freeze Dry System base unit Flat blade screwdriver or 5 16 socket and a 7 16 wrench or socket Remove the four plastic hole plugs from the top of the Freeze Dry System on which the Stoppering Tray Dryer is to be mounted If the Freeze Dry System has a flat gasket around the 3 0 inch vacuum port remove it Make sure the lower clamp provided on the vacuum coupling opposite the end connected to the Stoppering Tray Dryer chamber is loose Secure this clamp with tape or slide the clamp all the way up on the vacuum coupling and tighten it slightly to keep it from sliding down and coming off the coupling 7 4 20 X 314 HEX HEAD SCREWS 4 PLACES 1 4 FLA
19. 522 7658 International 816 333 8811 65 Appendix C Freeze Dryer Specifications Wiring Diagram Catalog 77530xx 77535xx 77540xx 79600xx and 77550xx 230V 50 or 60 Hz Models DLAGH AM FREEZE ORY 12 LITER CASCADE LABCONCO 2304 50 00 HI PEN 740550 SEW WIRING me 6 FREEZE DAT 6 1248 LITER SINGLE STAGE m EY fF 1 E D i wi ia oc E 66 Product Service Domestic 1 800 522 7658 International 816 333 8811 APPENDIX D FREEZE DRYER ACCESSORIES The following accessories are available for the Freeze Dryer PART DESCRIPTION 1467700 Vacuum Pump Two stage direct drive pump 195 liters minute 115 VAC 50 60 Hz single phase 7 8 amps Includes Pump Exhaust Filter 1473400 Catalog 1473400 7739403 Vacuum Pump Two stage direct drive pump 195 liters minute 230 VAC 50 60 Hz single phase 4 0 amps Includes Pump Exhaust Filter 1473400 Catalog 1473400 7439000 Vacuum Pump Two stage direct drive pump 173 liters minute 115 VAC 50 60 Hz single phase 5 8 amps Includes Pump Exhaust Filter Catalog 7670400 7439200 Vacuum Pump Two stage direct drive pump 173 liters minute 230 VAC 50 60 Hz single phase 2 9 amps Includes Pump Exhaust Filter Catalog 7670400 7769600 Vacuum Pump Chemical Resistant Two stage direct drive pump 173 liters minute 115 VAC 50 60 Hz single phase 5 8 amps Includes Pump Exhaust Filter Catalog 7670400 7769800 Vacuum Pump
20. 7934037 6 Liter Cascade Freeze Dryer 230 198 254 50 1 5 5 10 7934040 6 Liter Cascade Freeze Dryer 230 187 253 60 1 5 5 10 7934041 6 Liter Cascade Freeze Dryer 230 187 253 60 1 5 5 10 7934042 6 Liter Cascade Freeze Dryer 230 187 253 60 1 5 5 10 7934044 6 Liter Cascade Freeze Dryer 230 187 253 60 1 5 5 10 7934046 6 Liter Cascade Freeze Dryer 230 187 253 60 1 5 5 10 7934047 6 Liter Cascade Freeze Dryer 230 187 253 60 1 5 5 10 Product Service Domestic 1 800 522 7658 International 816 333 8811 61 Appendix C Freeze Dryer Specifications Voltage Amperage w o Catalog Operating Vacuum Max with Number Description Nominal Range Frequency Phase Pump Vacuum Pump 7754030 12 Liter Freeze Dryer 230 198 254 50 1 4 5 9 7754031 12 Liter Freeze Dryer 230 198 254 50 1 4 5 9 7754032 12 Liter Freeze Dryer 230 198 254 50 1 4 5 9 7754034 12 Liter Freeze Dryer 230 198 254 50 1 4 5 g 7754036 12 Liter Freeze Dryer 230 198 254 50 1 4 5 9 7754037 12 Liter Freeze Dryer 230 198 254 50 1 4 5 9 7754040 12 Liter Freeze Dryer 230 187 253 60 1 5 9 7754041 12 Liter Freeze Dryer 230 187 253 60 1 5 9 7754042 12 Liter Freeze Dryer 230 187 253 60 1 5 9 7754044 12 Liter Freeze Dryer 230 187 253 60 1 5 9 7754046 12 Liter Freeze Dryer 230 187 253 60 1 5 9 7754047 12 Liter Freeze Dryer 230 187 253 60 1 5 9 7960030 12 Liter Cascade Freeze Dryer 230 198 254 50 1 5 5 10 7960031 12 Liter Cascade Freeze Dryer 230 198 254 50 1 5 5 10 7960032 12 Liter Cascade Freeze Dryer 230 198 254 50
21. Chemical Resistant Two stage direct drive pump 173 liters minute 230 VAC 50 60 Hz single phase 2 9 amps Includes Pump Exhaust Filter Catalog 7670400 Product Service Domestic 1 800 522 7658 International 816 333 8811 67 Appendix D Freeze Dryer Accessories PART DESCRIPTION 1472200 Pump Inlet Filter Disposable filter that prevents oil back streaming and protects vacuum pump from sub micron particles Fits vacuum pumps 1466700 and 7739403 1473400 Pump Exhaust Filter Disposable filter that removes visible oil mist and odor from vacuum pump exhaust Fits vacuum pumps 1467700 and 7739403 1473200 Replacement Element Oil Mist Pump Exhaust Filter Fits pump exhaust filter 1473400 1473300 Replacement Element Odor Pump Exhaust Filter package of 5 Fits pump exhaust filter 1473400 or vacuum pumps 1467700 and 7739403 7670400 Replacement Filter Element Disposable filter that removes oil mist from the vacuum pump exhaust Fits vacuum pumps 7439000 7439200 7769600 and 7769800 1988000 Vacuum Pump Oil 1 Liter A molecularly distilled hydrocarbon oil with low vapor pressure For vacuum pumps 1467700 and 7739403 7772000 Soda Acid Trap Secondary trap that prevents migration of corrosive chemicals into vacuum pump 7772100 Replacement Media for Soda Acid Trap 7772700 Vacuum Pump Oil 1 Liter A mineral oil with low vapor pressure For vacuum pumps 7439000 7439200 77
22. Eye Contact Immediately flush eyes with fresh water for at least 15 minutes If irritation persists get medical attention Skin Contact Wash contaminated areas with soap and water Remove contaminated clothing and footwear Wash clothing before reuse Discard footwear which cannot be decontaminated Medical attention may be required Inhalation Remove patient to fresh air If breathing stops give artificial respiration Get medical attention immediately if required Ingestion Get medical attention immediately Do not induce vomiting Product Service Domestic 1 800 522 7658 International 816 333 8811 49 CHAPTER 8 Mopiryinc Your STOPPERING TRAY Dryer DisPLay Your Stoppering Tray Dryer has been carefully calibrated and tested before shipping however under certain circumstances it may be necessary to adjust the calibration of the vacuum display or to reset factory settings These adjustments may be necessary if the Stoppering Tray Dryer requires service An offset may be added to the vacuum display Use an accurate traceable reference to compare the readings Vacuum offset may be varied 0 010 mBar in 0 001 mBar increments Modifying the Display To enter an offset or to restore all factory settings perform the following steps e Press the DISPLAY button until the Set Up LED is lit e Press and hold DISPLAY button for 10 seconds The display will first show the screen used for setting Auto mode parameters and
23. In the event of a warranty claim contact Labconco Corporation or the dealer who sold you the product If the cause is determined to be a manufacturing fault the dealer or Labconco Corporation will repair or replace all defective parts to restore the unit to operation Under no circumstances shall Labconco Corporation be liable for indirect consequential or special damages of any kind This statement may be altered by a specific published amendment No individual has authorization to alter the provisions of this warranty policy or its amendments Lamps and filters are not covered by this warranty Damage due to corrosion or accidental breakage is also not covered Limitation of Liability The disposal and or emission of substances used in connection with this equipment may be governed by various federal state or local regulations All users of this equipment are required to become familiar with any regulations that apply in the user s area concerning the dumping of waste materials in or upon water land or air and to comply with such regulations Labconco Corporation is held harmless with respect to user s compliance with such regulations Contacting Labconco Corporation If you have questions that are not addressed in this manual or if you need technical RS assistance contact Labconco s Customer Service Department or Labconco s Product Service Department at 1 800 821 5525 or 1 816 333 8811 between the hours of 7 00 a m and 6 00 p m
24. Manual the status of the Stoppering Tray Dryer may be monitored simultaneously with the status of the Freeze Dryer Computer Connection for Computer Interface Check your computer to see which type of serial port is provided then use a connecting cable below 1 Computers with a 25 pin D sub male serial connector should use Connect Cable Labconco part number 7537801 to connect a computer to the Labconco Freeze Dryer 2 Computers with a 9 pin D sub male serial connector should use Connect Cable Labconco part number 7537800 to connect a computer to the Labconco Freeze Dryer The purpose of the RS232 interface is to send data to a data logging computer to monitor the state and activity of the Freeze Dryer This data is half duplex data The data properties are as follows Product Service Domestic 1 800 522 7658 International 816 333 8811 37 Chapter 6 Using the RS232 Receptacle Data Rate 2400 Baud 8 Bit word length 1 Start bit 1 Stop bit No parity is transmitted Standard ASCII character set Pino No The time between data transmissions may be varied by the user to occur at 10 30 60 300 or 600 second intervals Press the MENU button until the RS232 screen appears on the display RS 232 TRANSMISSION RATE 10 SECONDS Press select until the desired time interval is shown The format of the transmitted message is as follows B lt T 48 V 18 SF 999 C 999 PG 9 gt Where B Base Unit T Collecto
25. No Qty Description 1 7592002 1 Compressor 115V 60 Hz 7592001 1 Compressor 230V 50 Hz 7592000 1 Compressor 230V 60 Hz 2 7501900 1 Lexsol Pump 115V 7501901 1 Lexsol Pump 230V 3 7510900 1 Heater 115V 7510901 1 Heater 230V 4 7529500 1 Bulkhead Harness 5 7353300 1 Temperature Sensor System 6 7353301 3 Temperature Sensor Sample 7 7765500 1 Diaphragm 8 7354000 1 Door Gasket 9 1926200 20 Clip Door Gasket 10 7766801 2 Gal Heat Transfer Fluid Not Shown 11 7353500 1 Printed Circuit Board Control 12 7448000 1 Printed Circuit Board RS232 13 7761900 1 Coupling Vacuum 14 1966900 2 Clamp Coupling 15 7781502 1 Door Assembly Product Service Domestic 1 800 522 7658 International 816 333 8811 53 54 Appendix A Stoppering Tray Dryer Components Product Service Domestic 1 800 522 7658 International 816 333 8811 ApPENDIX B STOPPERING TRAY Dryer DIMENSIONS INCHES CENTIMETERS Product Service Domestic 1 800 522 7658 International 816 333 8811 55 Appendix B Stoppering Tray Dryer Dimensions Serum Bottle Capacity of the Stoppering Tray Dryer Size Labconco No Shelf Capacity No of Shelves Total Capacity 2 ml 7575010 399 3 1197 3 ml 7575210 296 3 888 5 ml 7573010 255 3 765 5 ml 7762310 255 3 765 10 ml 7573210 195 3 585 10 ml 7762610 255 3 765 20 ml 7573410 132 3 396 30 ml 7573610 86 3 258 50 ml 7573810 72 2 144 100 ml 7574010 42 2 84 125 ml 7574
26. freeze dry system one flask at a time so that the vacuum in the system may recover before adding another sample to the system If the vacuum does not recover the capacity of the freeze dry system has been exceeded and the sample should be removed If there is a problem with a particular type of sample melting when placed on the freeze dry system dilution of the sample with more water or providing some insulation around the flask to decrease the rate of heat absorption by the sample may help If the eutectic temperature of the sample is 40 to 60 C the freeze dry system selected for use must be equipped with cascade type refrigeration so that the collector temperature can be cooled to below 75 C or a dry ice solvent trap may be used between the collector and the vacuum pump Samples Containing Volatile Substances In certain cases the solvent in a sample to be freeze dried may contain volatile components such as acetonitrile methanol acetic acid formic acid or pyridine In addition to these substances having an effect on the eutectic temperature they may increase the vapor pressure at the surface of the sample Also compared to water they will require the absorption of less heat for sublimation to occur Hence samples that contain volatile substances will have a greater tendency to melt particularly when placed in flasks or exposed to room temperature If a sample containing a volatile substance tends to melt when placed on
27. helps you load samples easily and lyophilize efficiently How to select Lyph Lock Flasks for your Freeze Dry System Select the Lyph Lock Flasks based on your sample sizes Flasks should be filled to no more than one third of their volume so that maximum surface area is achieved and effi cient lyophilization is ensured A complete Lyph Lock Flask includes a glass top and bottom and a rubber ring seal Tops bottoms and seals are available separately as replacement components Adapters are required to attach flasks to freeze dry valve ports Flask Complete Complete Flask Flask Lyph Lock Flask Dimensions Size Flas Flas Top Top Seal Bottom Flask Bottom 19 38 STJ 24 40 STJ 19 38 STJ 20 40 ST HxID 25ml 7550000 75540 75520 7556000 75590 00 75570 00 37mmx 34mm 50ml 7550200 75542 15520 7556000 7559000 7557200 67mm x34mm 100ml 7550400 75544 15522 7556200 7559200 7557400 50 mm x 59 2 mm 250ml 7550600 75546 75522 7556200 7559200 7557600 110 mm x 59 2 mm 500ml 7550800 75548 15524 7556400 7559400 7557800 103 mm x 90 2 mm 50ml 7550900 75549 75524 7556400 7559400 7557900 145 mm x 90 2 mm 1000 ml 7551000 75550 1524 7556400 7559400 7558000 187 mm x 90 2 mm E PTYTYLLTYWYTHXHEBBR MB PE Appendix D Freeze Dryer Accessories Borosilicate glass adapters with either 19 38 or 24 40 standard taper joints have 90 bend Required order separately Only three pieces per flask no hooks or springs The co
28. important to remember these factors when trying to obtain efficient utilization of your freeze dry system A listing of selected materials and their approximate drying times are shown in Table 1 for your reference Table 1 SAFE TEMPERATURE AND DRYING TIMES FOR SELECTED MATERIALS Material Safe Collector Hours 10mm Thick Temperature Temperature Approx is Ze Milk 5 40 10 Urea 7 40 10 Blood Plasma 10 to 25 40 16 Serum 25 40 18 Vaccinia 30 to 40 50 22 Influenza Vaccine 30 50 24 Human Tissue 30 to 40 50 48 Vegetable Tissue 50 80 60 Total sample quantities are contingent on various freeze dryer capacities Up to the point of overloading the system the greater the surface area of the sample the faster the rate of freeze drying By contrast for a given surface area the thicker the sample the slower the rate of freeze drying This is based on the fact that the heat of sublimation is usually absorbed on one side of the frozen sample and must travel through the frozen layer to vaporize water at the other surface In addition as the sample is freeze dried the water vapor must travel through the layer of dried material The thicker the sample the greater the chance that the dried layer may collapse which would cause an additional decrease in the rate of freeze drying The surface area and thickness of the sample can usually be ignored when each sample contains on
29. inches of area provides heat control With RS232 output connection 7806033 Bulk Tray Dryer 230V 50 60 Hz Three shelves 630 square inches of area provides heat control With 6 port manifold and RS232 output connection 7948020 Stoppering Tray Dryer 115V 60 Hz three shelves 600 square inches of area provides temperature control and stoppering under vacuum 7948030 Stoppering Tray Dryer 230V 50 Hz three shelves 600 square inches of area provides temperature control and stoppering under vacuum 7948040 Stoppering Tray Dryer 230V 60 Hz three shelves 600 square inches of area provides temperature control and stoppering under vacuum 7726500 6 Port Manifold for use with Stoppering Tray Dryer Mounts between the Stoppering Tray Dryer and the base unit and provides 6 freeze dry valves 7537800 Cable Connect the RS232 output from the Freeze Dryer or Freeze Dryer Tray Dryer combination to an IBM compatible computer with a 9 pin serial data port 7537801 Cable Connects the RS232 output from the Freeze Dryer or Freeze Dryer Tray Dryer combination to an IBM compatible computer with a 25 pin serial data port 7761500 Isolation Valve Mounts between the Stoppering Tray Dryer and the base unit which provides a way to isolate the base unit vacuum system from the Stoppering Tray Dryer vacuum system 7390702 6L Baffle Mounts in the collector chamber to increase ice holding capacity when operating with vacuum control 7390701
30. increments of approximately 2 to 3V increments for 115V models or disabled Low line limit may be lowered in 5 increments of approximately 4 to 5V increments for 230V models or disabled High line limit may be raised in 5 increments of approximately 2 to 3V increments for 115V models or disabled High line limit may be raised in 5 increments of approximately 4 to 5V increments for 230V models or disabled Moisture Sensor Alarm The moisture sensor alarm may be disabled It is shipped enabled as the factory default setting Modifying the Display To enter an offset or to configure the alarms perform the following steps Press and hold MENU button approximately 10 seconds until the display shows PRODUCTION MENU MASTER RESET It is recommended that you do NOT perform a Master Reset because all offsets and configurations that have been entered will be lost If you must perform a Master Reset hold SELECT approximately 5 seconds This will reset Vacuum units to mBar Vacuum set point to 0 mBar Temperature units to C Refrigeration total hours to 0 Vacuum pump total hours to 0 RS232 transmission rate to 10 seconds Temperature offset to 0 C Vacuum offset to 0 mBar Low line voltage to 0 V offset Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 8 Modifying Your Freeze Dryer Display High line voltage to 0 V offset Moisture sensor to enabled Refrigeration to operate i
31. plastic knob on the valve to vent 28 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 4 Using Your Freeze Dryer position The sample container may now be removed In the vent position the bevel on the valve knob should point away from the sample port Ampules may be flame sealed while connected to a valve by using a sealing torch Care must be taken not to burn the valve An insulation material placed between the valve and the torch is recommended Shut Down At the end of a run or when a sufficient amount of condensate accumulates on the collector coil to obstruct the flow of vapor to the collector chamber the Freeze Dryer should be defrosted First release system vacuum by turning the plastic knob on a valve to the open position or by pulling the collector chamber drain plug out of the drain hose Now press the Vacuum Switch on the control panel to turn the vacuum pump OFF Press the Refrigeration Switch next to the illuminated LED to turn OFF the refrigeration system Turn OFF the Main Power Switch on the left hand side of the cabinet After a run is complete it may be desirable to purge contaminants from the vacuum pump oil This can be accomplished by first closing the purge valve by pressing the purge switch The LED will illuminate Then turn on the vacuum pump by pressing the vacuum switch let the pump operate for an extended period of time Defrosting The following procedure should be
32. section of this manual and of the manual supplied with the Freeze Dry System Venting the Vacuum Pump If any materials will be placed in the Stoppering Tray Dryer that can liberate hazardous gases when heated the vacuum pump exhaust must be vented to a fume hood or other ventilation device Electrical Connection Plug the power cord into the receptacle on the back of the Stoppering Tray Dryer and plug the other end into a suitable power receptacle 13 DO NOT ATTEMPT TO PLUG THE STOPPERING TRAY DRYER INTO THE FREEZONE FREEZE DRY SYSTEM 12 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 3 Getting Started CAUTION When the appropriate power cord is plugged into the power receptacle on the rear panel of the tray dryer the clamp on the tray dryer receptacle should be tightened to prevent the cord from accidentally being switched with the freeze dryer cord located underneath the tray dryer The freeze dryer may require different mains A C voltage and switching these power cords may cause damage Chemical Resistance of Freeze Dryer Components The FreeZone Freeze Dry System and Stoppering Tray Dryer are designed to be chemically resistant to most compounds that are commonly used in freeze drying processes However by necessity the Freeze Dryer is comprised of a number of different materials some of which may be attacked and degraded by certain chemicals The degree of degradation is depend
33. serum bottles under original vacu um The stopper and serum bottle are inserted into the adapter body and lyophilization begins After the process is completed the researcher slides the stopper into position so when the valve is turned from vacuum to vent the serum bottle is tightly sealed by the stopper The ejector tube is then used to force the serum bottle out of the adapter Shipping weight 1 Ib 0 4 kg Stoppering Adapter Body Serum Bottle Valve Port Z Vent Hole Ejector Tube Stopper 74 Product Service Domestic 1 800 522 7658 International 816 333 8811 Ampules Labconco Ampules are fabricated of highest quality borosili cate glass for strength and durability They are available in five different configurations to provide the ideal ampule for your specific lyophilization requirements from tray drying to flame sealing applications Ampules Ampules are supplied in packages of 100 Size Straight Bulb Type Pre Scored Round Stoppering Flat Bottom Bottom I ml 7572710 7570010 7570610 2 ml 7570810 7572310 4ml 7572810 5ml 7570210 7571010 10 ml 7571210 7571610 25 ml 7571810 50 ml 7572010 Appendix D Freeze Dryer Accessories Accessories a Oxygen Natural Gas Sealing Torch 7578500 Torch specifically designed for flame sealing freeze dry ampules Seals all types of heat resistant glass Connects to natural gas butane or propane and oxygen with 1 4 ID hose connectors Shipping weight 3 Ib
34. the actual temperature of the collector When the vacuum in the system is above 5 mBar the vacuum display will indicate HI At 5 mBar and below the display will show the actual vacuum When the system vacuum is between 0 450 and 0 133 mBar the lower green vacuum graph LED will flash When the system vacuum level is lt 0 133 mBar the green LED will be lit steadily indicating that most samples may be added Automatic Start Up Models equipped with a purge valve To run the Auto Mode press the panel switch labeled REFRIGERATION AUTO The green LED above the switch will illuminate The LED s above the vacuum and purge switches will also illuminate The refrigeration system and vacuum pump will start and the purge valve will close When the collector reaches 40 C the purge valve will open The Temperature and Vacuum Graphs will indicate collector temperature and system vacuum The LCD display will show the actual temperature of the collector When the vacuum in the system is above 5 mBar the vacuum display will indicate HI At 5 mBar and below the display will show the actual vacuum When the system vacuum is between 0 450 and 0 133 mBar the lower green vacuum graph LED will flash When the system vacuum level is lt 0 133 mBar the green LED will be lit steadily indicating that most samples may be added Product Service Domestic 1 800 522 7658 International 816 333 8811 25 Chapter 4 Using Your Freeze Dryer Manua
35. then will show PRODUCTION MENU MASTER RESET Product Service Domestic 1 800 522 7658 International 816 333 881 1 Chapter 8 Modifying Your Stoppering Tray Dryer Display If you want to restore all factory settings hold ENTER approximately 5 seconds This will reset Vacuum units to mBar Temperature units to C Refrigeration service hours to 0 Refrigeration total hours to 0 RS232 transmission rate to 10 seconds Vacuum offset to O mBar At the completion of Master Reset the display will show operational parameters If you do not want to restore all factory settings but want to adjust the vacuum offset press DISPLAY briefly and the display will show VACUUM OFFSET O mBar Press ft or amp until the appropriate offset is shown Each number represents an offset of 0 001 mBar Press DISPLAY and the display will show PRODUCTION MENU MASTER RESET Wait approximately 10 seconds and the display will default to show operational Product Service Domestic 1 800 522 7658 International 816 333 8811 51 APPENDIX STOPPERING TRAY DRYER COMPONENTS The following pages list components that are available for your Stoppering Tray Dryer The parts shown are the most common replacement parts If other parts are required contact Product Service 52 Product Service Domestic 1 800 522 7658 International 816 333 8811 Appendix A Stoppering Tray Dryer Components Item Part
36. to a maximum height of 107 mm 4 2 inches Minimum serum bottle height with lowered stopper for a 2 shelf system is 56 mm 2 2 inches For a single shelf system raise both the top and middle shelves until they latch in place in their top positions The spacing for a single shelf system will accommodate a bottle with raised stopper up to a maximum height of 196 mm 7 7 inches and the minimum height of a bottle with lowered stopper for successful stoppering is 114 mm 4 5 inches To unlatch the shelves press the latch protruding from the side of the shelf support structure and move the latch until it clears the shelf and allows the shelf to drop The top shelf has one latched position the middle shelf has two latched positions and the bottom shelf should not latch in any position Product Service Domestic 1 800 522 7658 International 816 333 8811 27 Chapter 4 Using Your Stoppering Tray Dryer Shelf Loading The stoppering mechanism is capable of generating a very strong force which can damage the shelves or mechanism Therefore it is important to distribute the serum bottles to be stoppered evenly across the entire surface of each shelf Your Stoppering Tray Dryer has a unique system for keeping the shelves level and moving smoothly while stoppering If a problem occurs during stoppering the system is designed to flex a small amount to lessen the possibility of damage to the unit The stoppering action should be monit
37. 0 522 7658 International 816 333 8811 25 Chapter 4 Using Your Stoppering Tray Dryer Changing the Program Parameters in the Middle of a Run 1 2 3 4 5 Press DISPLAY to obtain Monitor screen Note current operating segment Press DISPLAY to obtain Auto screen Enter a segment number that will occur after the current segment that is running The presently running segment cannot be modified while the system is running Modify as required Press ENTER Stopping the Freeze Dry Cycle 1 At the end of the last programmed segment the freeze dry system will automatically stop The refrigeration system and the heater will shut off The display will show Segment E End To stop before the completion of the last programmed segment press RUN STOP The amber lamp will turn off as will the refrigeration system and heater The display will remain active but time functions will stop operating The entire system can be shut off by pressing the Power Switch If the Power switch is shut off prior to stopping the cycle with the RUN STOP button when the Power Switch is again turned on the system will resume operation and attempt to complete the programmed cycle from the point at which it was shut off The display mode indicator PROGRAM will flash to indicate power loss during programmed run Monitoring the System Operation Press the Display button until the monitor LED lights The display will s
38. 1 Introduction pressure and ultimately overloads the collector and vacuum pump Samples that have eutectic temperatures of 20 C or lower should be placed on the freeze dry system one flask at a time so that the vacuum in the system may recover before adding another sample to the system If the vacuum does not recover the capacity of the freeze dry system has been exceeded and the sample should be removed If there is a problem with a particular type of sample melting when placed on the freeze dry system dilution of the sample with more water or providing some insulation around the flask to decrease the rate of heat absorption by the sample may help If the eutectic temperature of the sample is 40 to 60 C the freeze dry system selected for use must be equipped with cascade type refrigeration so that the collector temperature can be cooled to below 75 C or a dry ice solvent trap may be used between the collector and the vacuum pump Samples Containing Volatile Substances In certain cases the solvent in a sample to be freeze dried may contain volatile components such as acetonitrile methanol acetic acid formic acid or pyridine In addition to these substances having an effect on the eutectic temperature they may increase the vapor pressure at the surface of the sample Also compared to water they will require the absorption of less heat for sublimation to occur Hence samples that contain volatile substances will have
39. 1 5 5 10 7960034 12 Liter Cascade Freeze Dryer 230 198 254 50 1 5 5 10 7960036 12 Liter Cascade Freeze Dryer 230 198 254 50 1 5 5 10 7960037 12 Liter Cascade Freeze Dryer 230 198 254 50 1 5 5 10 7960040 12 Liter Cascade Freeze Dryer 230 187 253 60 1 6 5 11 7960041 12 Liter Cascade Freeze Dryer 230 187 253 60 1 6 5 11 7960042 12 Liter Cascade Freeze Dryer 230 187 253 60 1 6 5 11 7960044 12 Liter Cascade Freeze Dryer 230 187 253 60 1 6 5 11 7960046 12 Liter Cascade Freeze Dryer 230 187 253 60 1 6 5 11 7960047 12 Liter Cascade Freeze Dryer 230 187 253 60 1 6 5 11 7755030 18 Liter Freeze Dryer 230 198 254 50 1 5 5 10 7755031 18 Liter Freeze Dryer 230 198 254 50 1 5 5 10 7755032 18 Liter Freeze Dryer 230 198 254 50 1 5 5 10 7755034 18 Liter Freeze Dryer 230 198 254 50 1 5 5 10 7755036 18 Liter Freeze Dryer 230 198 254 50 1 5 5 10 7755037 18 Liter Freeze Dryer 230 198 254 50 1 5 5 10 7755040 18 Liter Freeze Dryer 230 187 253 60 1 5 5 10 7755041 18 Liter Freeze Dryer 230 187 253 60 1 5 5 10 7755042 18 Liter Freeze Dryer 230 187 253 60 1 5 5 10 7755044 18 Liter Freeze Dryer 230 187 253 60 1 5 5 10 7755046 18 Liter Freeze Dryer 230 187 253 60 1 5 5 10 7755047 18 Liter Freeze Dryer 230 187 253 60 1 5 5 10 62 Product Service Domestic 1 800 522 7658 International 816 333 8811 Appendix C Freeze Dryer Specifications Environmental Conditions Indoor use only Maximum altitude 6562 feet 2000 meters Ambient temperature range 41 to 104 F 5
40. 12L Baffle Mounts in the collector chamber to increase ice holding capacity when operating with vacuum control Product Service Domestic 1 800 522 7658 International 816 333 8811 71 Appendix D Freeze Dryer Accessories Fast Freeze Flasks Fast Freeze Flasks are specially designed to be easier to handle faster to load and more convenient to use than other freeze dry glassware now in your laboratory Compatible with all major brands of laboratory freeze dry equipment Fast Freeze Flasks eliminate the risk of contamination from vacuum grease reduce spillage of valuable samples and require no washers gaskets or retainers How to select Fast Freeze Flasks for your Freeze Dry System Select Fast Freeze Flasks based on your sample sizes Flasks should be filled no more than one third of their volume so that maximum surface area is achieved and efficient lyophilization is assured A complete Fast Freeze Flask includes a rubber top glass bottom and a supply of filter paper Tops bottoms and filter paper are available separate ly as replacement components Adapters are required to attach flasks to freeze dry valve ports Flask Size 40 ml 80 ml 120 ml 150 ml 300 ml 600 ml 900 ml 1200 ml 2000 ml Complete Flask 7540000 7540200 7540300 7540400 7540600 7540800 7540900 7541000 7541200 Flask Bottom 7542000 7542200 7542300 7542400 7542600
41. 210 36 1 36 56 Product Service Domestic 1 800 522 7658 International 816 333 8811 AppENDIX C STOPPERING TRAY DRYER SPECIFICATIONS This Appendix contains technical information about the Freeze Dryer including electrical specifications environmental operating conditions and wiring diagrams Voltage Catalog Operating Number Description Nominal Range Frequency Phase Amperage 7948020 Stoppering Tray Dryer 115 103 127 60 1 12 4 100 90 110 50 1 12 4 7948030 Stoppering Tray Dryer 230 198 254 50 1 6 9 7948040 Stoppering Tray Dryer 230 187 253 60 1 6 9 Environmental Conditions Indoor use only Maximum altitude 6562 feet 2000 meters Ambient temperature range 41 to 104 F 5 to 40 C Maximum relative humidity 80 for temperatures up to 88 F 31 C decreasing linearly to 50 relative humidity at 104 F 40 C Main supply voltage fluctuations not to exceed 10 of the nominal voltage Transient over voltages according to Installation Categories II Over voltage Categories per IEC 1010 Temporary voltage spikes on the AC input line that may be as high as 1500V for 115V models and 2500V for 230V models are allowed Used in an environment of Pollution degrees 2 i e where normally only non conductive atmospheres are present Occasionally however a temporary conductivity caused by condensation must be expected in accordance with IEC 664 Product Service Domestic 1 800 522 7658 International 816 3
42. 33 8811 57 Appendix C Stoppering Tray Dryer Specifications Catalog 7948020 115V 60 Hz Diagram iring W WAIN DOZESCZ N d Sais ZHOS AOOL ZH 09 ASL ONINMW M l YJAY0 AVL NiIYJddOlS w 038 A S HE 479 38 AVAIVIT ONIMIM OONOOGYV 1 ooresed N d BOSNIS NILSAS 1 398N0s 83 o E e hoeeser N d SHOSNIS 373HS E 440 NO HIMOd NIVIN gt So 8 aw AFA AARAAATA 0056754 N d NHL SS d Lou vOvesed N d 1 1 1 1 00 CSCL N d SSINHYH PSS nse D0PSSEL N d IUNSOTONA corer N d LINN 3S 8 OL 831 3H 10SX37 Product Service Domestic 1 800 522 7658 International 816 333 8811 58 Appendix C Stoppering Tray Dryer Specifications Wiring Diagram Catalog 7948030 and 7948040 230V 50 or 60 Hz Models WARY LOZEGEL N d 3 OL won ZH 09 05 A0 amp Z ANINYY M YJAXO AVYL NIXJddOLlS WYX VIQ NIXIM O NOQ9gY oorestz N d BOSNIS W31SAS T N 3984N0S YIMOd c WESSE n d SYOSNIS J73HS 430 NO HIMOd NIVN 0056TSZ N d NAHI Ssvd procter OPESEL N d ABRIL AN Yh LOPEGEL N d SSINHYH LOYSSEL N d IYNSOTINI ooreie N d ZOLBZSE N d UNN 3SV8 OL x yan s Li eoresee N d 2 se pa dis dE a Po eos 59 Product Service Domestic 1 800 522 7658 International 816 333 8811 APPENDIX D STOPPERING TRAY DRYER ACCESSORIES The following accessories are available for the Freeze Dryer
43. 333 8811 Chapter 4 Using Your Stoppering Tray Dryer TEMPERATURE SENSOR X CALIBRATION ERROR Where X is S for the system probe 1 for sample probe 1 2 for sample probe 2 3 for sample probe 3 If this alarm occurs the faulty probe must be replaced If any of the sample probes are faulty it may be unplugged and the Stoppering Tray Dryer may be used The sample temperature display will show If the system probe is faulty it must be replaced before the Stoppering Tray Dryer can be used Product Service Domestic 1 800 522 7658 International 816 333 8811 31 32 CHAPTER 5 MAINTAINING YOUR STOPPERING TRAY DRYER Under normal operation the Stoppering Tray Dryer requires little maintenance The following maintenance schedule is recommended As needed l The user has the responsibility for carrying out appropriate decontamination if hazardous material is spilled on or inside the equipment This may be done by wiping the contaminated surfaces with a soft cloth dampened with alcohol Alcohol may craze the acrylic door Before using any cleaning or decontamination method except those recommended by Labconco users should check with Labconco that the proposed method will not damage the equipment Clean up all spills remove liquids from the chamber Clean door and gasket using soft cloth sponge or chamois and a mild non abrasive soap or detergent Check oil level of the vacuum pump It should be bet
44. 34034 6 Liter Cascade Freeze Dryer 230 50 x x 7934036 6 Liter Cascade Freeze Dryer 230 50 x x 7934037 6 Liter Cascade Freeze Dryer 230 50 x x x 7934040 6 Liter Cascade Freeze Dryer 230 60 7934041 6 Liter Cascade Freeze Dryer 230 60 x 7934042 6 Liter Cascade Freeze Dryer 230 60 x 7934044 6 Liter Cascade Freeze Dryer 230 60 x x 7934046 6 Liter Cascade Freeze Dryer 230 60 x x 7934047 6 Liter Cascade Freeze Dryer 230 60 x x x 7754030 12 Liter Freeze Dryer 230 50 7754031 12 Liter Freeze Dryer 230 50 x 7754032 12 Liter Freeze Dryer 230 50 x 7754034 12 Liter Freeze Dryer 230 50 X x 7754036 12 Liter Freeze Dryer 230 50 x x 7754037 12 Liter Freeze Dryer 230 50 x x x 7754040 12 Liter Freeze Dryer 230 60 7754041 12 Liter Freeze Dryer 230 60 x 7754042 12 Liter Freeze Dryer 230 60 x 7754044 12 Liter Freeze Dryer 230 60 x x 7754046 12 Liter Freeze Dryer 230 60 x x 7754047 12 Liter Freeze Dryer 230 60 x x x 7960030 12 Liter Cascade Freeze Dryer 230 50 7960031 12 Liter Cascade Freeze Dryer 230 50 x 7960032 12 Liter Cascade Freeze Dryer 230 50 x 7960034 12 Liter Cascade Freeze Dryer 230 50 x x 7960036 12 Liter Cascade Freeze Dryer 230 50 x x 7960037 12 Liter Cascade Freeze Dryer 230 50 x x x 7960040 12 Liter Cascade Freeze Dryer 230 60 7960041 12 Liter Cascade Freeze Dryer 230 60 x 7960042 12 Liter Cascade Freeze Dryer 230 60 x 7960044 12 Liter Cascade Freeze Dryer 230 60 x x 7960046 12 Liter Cascad
45. 522 7658 International 816 333 8811 Chapter 4 Using Your Stoppering Tray Dryer program to allow the identical protocol to be repeated by simply pushing the RUN button A typical 3 segment program is shown in Figure 5 mocasa gt oamutama SEGMENT FREEZING PRIMARY SECONDARY DRYING DRYING Automatic Start Up of Freeze Dryer Vacuum At the end of Segment 1 Hold if the StopperingTray Dyer is connected to the Freeze Dry System base unit the vacuum provided by the Freeze Dryer will start automatically The base unit should have the refrigeration started in manual mode to allow it to reach temperature while the Tray Dryer is processing Segment 1 of the program Do not start the base unit s refrigeration using automatic mode This will not allow the Tray Dryer to start the vacuum on the Freeze Dryer Connect the Tray Dryer to the Freeze Dryer with cable 7353403 this cable is shipped with the Tray Dryer One end of the cable plugs into the 4 pin connector Output to Freeze Dryer on the back of the Tray Dryer in the lower right hand corner of the unit when viewing the back of the unit and the other end of the cable plugs into the 4 pin connector Stoppering Tray Dryer Input on the back of the Freeze Dryer in the upper right hand corner of the unit when viewing the back of the unit Product Service Domestic 1 800 522 7658 International 816 333 8811 23 Chapter 4 Using Your Stoppering Tray Dryer Programmin
46. 69600 7769800 7772500 Carbon Solvent Trap Secondary trap that prevents migration of organic solvents into vacuum pump 7772600 Replacement Activated Carbon Media for Carbon Solvent Trap 68 Product Service Domestic 1 800 522 7658 International 816 333 8811 Appendix D Freeze Dryer Accessories PART DESCRIPTION 7538000 Secondary Vacuum Cold Trap Provides additional protection for the vacuum pump when processing low eutectic samples 9 34 high x 7 7 8 diameter 304 stainless steel with 34 vacuum connections For use with dry ice and solvent Cools to approximately 75 C 7522800 12 Port Drying Chamber 9 high x 7 7 8 diameter 304 stainless steel with 12 freeze dry valves 7522900 16 Port Drying Chamber 13 high x 138 diameter 304 stainless steel with 16 freeze dry valves 7443500 Clear Drying Chamber with 8 Valves For bulk drying or drying in flasks 9 0 Dia 7444000 Clear Drying Chamber with 8 Valves For bulk drying or drying in flasks 12 0 Dia 7442900 Clearing Drying Chamber For bulk drying 9 0 Dia 7867000 Clear Drying Chamber For Bulk Drying 12 0 Dia 7521000 Heated Drying Chamber 10 4 high x 9 diameter type 304 stainless steel The 3 shelf product heaters heat to 43 C 110 F 115V 7521001 Heated Drying Chamber 10 4 high x 9 diameter type 304 stainless steel The 3 shelf product heaters heat to 43 C 110 F 230V 7509200 Product Heater For use in chamber 7522
47. 800 Provides 3 heated shelves operating at 43 C 110 F 115V 7509201 Product Heater For use in chamber 7522800 Provides 3 heated shelves operating at 43 C 110 F 230V 7442100 Drying Rack Unheated Provides three shelves For use in chambers 7443500 and 7522800 7441700 Drying Rack Unheated Provides three shelves for use in chambers 7444000 7867000 7522900 7522300 20 Port Manifold 10 high x 27 2 wide x 8 5 8 deep Type 304 stainless steel manifold with 20 freeze dry valves Product Service Domestic 1 800 522 7658 International 816 333 8811 69 Appendix D Freeze Dryer Accessories PART DESCRIPTION 7522400 10 Port Manifold with support shelf 10 high x 26 wide x 6 5 8 deep Type 304 Stainless Steel Manifold with 10 Freeze Dry Valves amp 1 Shelf 7522500 20 Port Manifold with support shelves 10 high x 26 wide x 9 1 2 deep Type 304 Stainless Steel Manifold with 20 Freeze Dry valves and 2 shelves 7868500 48 Port Ampule Manifold 28 5 8 high x 5 wide x 5 deep Type 304 stainless steel with 48 each 4 tube stems 7509600 Sample Valve Kit Includes neoprene valve body knob and installation parts 7439902 Glass Collector Chamber Lid For use with solvlents that attack the acrylic lid 7439902 Glass Collector Chamber Lid For use with solvlents that attack the acrylic lid 7509300 Product Heater For use in chambe
48. 994 30 gt B lt T 8O0V L amp SF 9990 999PG 9 gt TD lt PR 18 IRTR 1 ST 26P1 25P2 999P3 999 30 gt B lt T 80V 14 SF 999C 999PG 9 gt TD lt PR 1S 1RTR 1OST 26P1 25P2 999PS 999 30 gt Bcl SUV 14 I 999C 999PG 9 UC R LS IRIR 10S 26P1 25P2 999P3 999N 3D CHAPTER 7 TROUBLESHOOTING Refer to the following if your Freeze Dry System fails to operate properly If the suggested corrective actions do not solve your problem contact Labconco for additional assistance FreeZone Freeze Dry Systems that are clean and dry and without samples attached should reach a vacuum of 0 133 mBar within 30 minutes and should achieve an ultimate vacuum of 0 033 mBar within 18 hours when the refrigeration is operating If the Freeze Dry System does not obtain a satisfactory vacuum perform the following maintenance tests I Vacuum Pump First make sure that the vacuum pump operates If it fails to operate check the electrical connections of the Freeze Dry System to the power source and then check the electrical connection of the vacuum pump to the Freeze Dry System If the vacuum pump has a power switch make sure that it is turned on If the vacuum is not adequate when the vacuum pump is operating proceed with the following steps 1 Check the oil and ensure it is clear and clean If the oil looks cloudy or has any particulates replace the pump oil Sometimes it may be necessary to flush the pump with clean oil several times T
49. Automatic Mode the purge valve and vacuum pump will operate automatically to perform this function In the Manual Mode the user must manually activate the purge valve and vacuum pump to perform this function During shut down the vacuum pump can be run for several minutes with the purge valve closed This will allow the warm pump oil to evaporate and expel solvent vapors that condensed in the pump oil during the freeze dry process Whether the Freeze Dryer is run in the Automatic Mode or the Manual Mode the user must manually activate the purge valve and vacuum pump to perform this function If power to the Freeze Dryer is interrupted during the freeze dry process the purge valve will open during the power outage and the vacuum bleed valve will open to allow atmospheric air to enter the system Operating the Freeze Dryer Set Up The Freeze Dryer may be configured to automatically start the vacuum pump when the collector temperature reaches 40 C The display units for vacuum may be selected to be mBar Pascal Pa or Torr and the temperature may be displayed as F or C The run time of the refrigeration system and the vacuum pump may be monitored To configure your Freeze Dryer turn the main power switch ON and press MENU The display will show VACUUM UNITS mBar Pa e Press SELECT until the desired units are flashing e Press MENU e The display will show VACUUM SET POINT XXXX YYY Where YYY is the units selec
50. Copyright 2004 Labconco Corporation All rights reserved Labconco Corporation 8811 Prospect Avenue Kansas City Missouri 64132 The information contained in this manual and the accompanying product are copyrighted and all rights are reserved by Labconco Corporation Labconco Corporation reserves the right to make periodic design changes without obligation to notify any person or entity of such change FreeZone is a registered trademark of Labconco Corporation Warranty Labconco provides a warranty on all parts and factory workmanship The warranty includes areas of defective material and workmanship provided such defect results from normal and proper use of the equipment The warranty for all Labconco products will expire one year from date of installation or two years from date of shipment from Labconco whichever is sooner except the following e Purifier Delta Series Biological Safety Cabinets and PuriCare Lab Animal Products carry a three year warranty from date of installation or four years from date of shipment from Labconco whichever is sooner e Steamscrubber amp FlaskScrubber Glassware Washers carry a two year warranty from date of installation or three years from date of shipment from Labconco whichever is sooner e Carts carry a lifetime warranty e Glassware is not warranted from breakage when dropped or mishandled This limited warranty covers parts and labor but not transportation and insurance charges
51. D SELECT TO CLEAR IT Press and hold SELECT for five seconds until the error message is cleared from the display Product Service Domestic 1 800 522 7658 International 816 333 8811 33 Chapter 4 Using Your Freeze Dryer Service Vacuum Pump The vacuum pump normally plugs into the vacuum pump electrical receptacle on the back of the Freeze Dryer When the Freeze Dryer has accumulated a total of 1000 operating hours the alarm indicator will flash Press MENU to display the alarm CHANGE VACUUM OIL HOLD SELECT TO CLEAR IT Press and hold SELECT for five seconds until the error message is cleared from the display This will reset the 1000 hour timer It may be necessary to service the vacuum pump more frequently than every 1000 hours depending on the operation of the Freeze Dryer The pump oil should be regularly monitored to verify that it is clean Moisture in Collector If there is liquid in the collector chamber and either a REFRIGERATION button or the VACUUM button is pressed neither function will start and an alarm will be activated When MENU is pressed the display will show MOISTURE IN COLLECTOR When the collector is drained the alarm will self cancel This feature prevents the inadvertent start of the vacuum pump when liquid is in the collector and thereby can extend the life of the vacuum pump A few drops of liquid may remain in the drain hose after draining When the vacuum pump is started these drops may b
52. France Belgique Belgi Fisher t l 0388671414 t l 056260260 Bioblock Scientific 0388671168 fax 056260270 email infos bioblock fr email belgium bioblock com Parc d innovation BP 50111 F67403 illkirch cedex www bioblock com www bioblock be Mode demploi Espa a tfno 915159234 fax 91 515 92 35 email ventas bioblock com www es fishersci com User s Manual FreeZone 6 12 and 18 Liter Freeze Dry Systems Models 7753020 7753522 7754030 7755030 7934020 7960030 7753021 7753524 7754031 7755031 7934021 7960031 7753022 7753532 7754032 7755032 7934022 7960032 7753024 7753534 7754034 7755034 7934024 7960034 7753026 7753542 7754036 7755036 7934026 7960036 7753027 7753544 7754037 7755037 7934027 7960037 7753030 7754040 7755040 7934030 7960040 7753031 7754041 7755041 7934031 7960041 7753032 7754042 7755042 7934032 7960042 7753034 7754044 7755044 7934034 7960044 7753036 7754046 7755046 7934036 7960046 7753037 7754047 7755047 7934037 7960047 7753040 7934040 7753041 7934041 7753042 7934042 7753044 7934044 7753046 7934046 7753047 7934047 LABCONCO CORPORATION 8811 PROSPECT AVENUE KANSAS CITY MO 64132 2696 800 821 5525 816 333 8811 FAX 816 363 0130 E MAIL labconco labconco com HOME PAGE www labconco com Register your product online at www labconco com productreg html gt A or return the attached card and receive FREE LabbyWear Labconco s Mascot Labby the LABster Copyright Information
53. ITHOUT THE PRIOR AUTHORIZATION OF LABCONCO UNAUTHORIZED RETURNS WILL NOT BE ACCEPTED Product Service Domestic 1 800 522 7658 International 816 333 8811 The United States Interstate Commerce Commission rules require that claims be filed with the delivery carrier within fifteen 15 days of delivery Chapter 3 Getting Started IF YOUR FREEZE DRYER WAS DAMAGED IN TRANSIT YOU MUST FILE A CLAIM DIRECTLY WITH THE FREIGHT CARRIER LABCONCO CORPORATION AND ITS DEALERS ARE NOT RESPONSIBLE FOR SHIPPING DAMAGE DO NOT DISCARD THE CARTON OR 13 PACKING MATERIAL FOR YOUR FREEZE DRYER UNTIL YOU HAVE CHECKED ALL OF THE COMPONENTS AND INSTALLED AND TESTED THE FREEZE DRYER Freeze Dryer Components Locate the model of Freeze Dryer you received in the following table Verify that the components listed are present and undamaged Catalog Numbers 6 12 and 18 Liter Console Models Teflon Catalog Coated Purge Drying Shell Number Description Volts Hz Chamber Valve Chamber Freezer 7753020 6 Liter Freeze Dryer 115 60 7753021 6 Liter Freeze Dryer 115 60 x 7753022 6 Liter Freeze Dryer 115 60 x 7753024 6 Liter Freeze Dryer 115 60 x x 7753026 6 Liter Freeze Dryer 115 60 x x 7753027 6 Liter Freeze Dryer 115 60 x x x 7753030 6 Liter Freeze Dryer 230 50 7753031 6 Liter Freeze Dryer 230 50 x 7753032 6 Liter Freeze Dryer 230 50 x 7753034 6 Liter Freeze Dr
54. In this mode the vacuum pump will start when the collector temperature reaches 40 C Vacuum Graph Display This display indicates the relative system vacuum level The highest LED indicates that the vacuum level is above 2 0 mBar The indicators will sequence down when the vacuum level reaches 2 0 1 0 0 8 0 6 0 45 0 12 mBar The lower green LED flashes when the system vacuum level is 0 45 to 0 12 mBar and illuminates steadily below 0 133 mBar Collector Temperature Graph Display This display indicates the temperature of the collector The highest LED indicates the collector temperature is warmer than 10 C The indicators will sequence down when the temperature reaches 10 0 10 20 30 40 C When the collector temperature is 40 C or lower the green indicator will light Alarm Indicator This red LED indicates that a system alarm has occurred Press the Menu Switch to display the alarm message on the LCD display Main Power Switch Turns the Freeze Dryer on or off Not shown located on the left side of the cabinet Defrost Switch Used to defrost ice from the collector coil Defrost Indicator This green LED illuminates when the Freeze Dryer is in defrost mode Purge Valve Switch Used to open or close the purge valve if the model is so equipped Purge Valve Indicator This green LED illuminates when the purge valve is closed Shell Freezer Vacuum Chamber Switch Used to operate the shel
55. R CHAPTER 6 USING THE RS232 RECEPTACLE Computer Connection for Computer Interface CHAPTER 7 TROUBLESHOOTING Vacuum Pump Gaskets Tubing Connections Sample Valves System Components amp Collection Chamber Isolation Refrigeration Module Operation 27 27 28 29 29 30 31 32 32 33 33 34 34 35 37 37 42 42 43 45 48 CHAPTER 8 MODIFYING YOUR FREEZE DRYER DISPLAY 49 Temperature amp Vacuum Display Line Voltage Alarm Points Moisture Sensor Alarm Modifying the Display APPENDIX A FREEZE DRYER COMPONENTS APPENDIX B FREEZE DRYER DIMENSIONS APPENDIX C FREEZE DRYER SPECIFICATIONS Electrical Specifications Environmental Conditions Wiring Diagrams APPENDIX D FREEZE DRYER ACCESSORIES DECLARATION OF CONFORMITY 49 49 50 50 54 59 60 60 63 64 67 76 CHAPTER 1 INTRODUCTION Congratulations on your purchase of a Labconco FreeZone Freeze Dry System which is designed for laboratory lyophilization procedures The refrigerant used in the refrigeration system is CFC free so it will not endanger the environment The unit is easy to install and maintain Proper care and maintenance of this product will result in many years of dependable service Freeze Dry Process Freeze drying is an important process in sample preparation and for the preservation and storage of biologicals pharmaceuticals and foods Of the various methods of dehydration freeze drying lyophilization is especially suited for
56. SERVICE HOURS e Press to reset the Service Hours to 0 This allows you to keep track of the time the refrigeration system operated since it was serviced e The display will show REFRIGERATION TOTAL HOURS XXXX RESET SERVICE HOUR X e Hold for 5 seconds e Press ENTER e Atany time the DISPLAY button can be pressed to select a different display screen Manual Control Operation 1 Turn the Power switch ON The display will become active 2 Push the DISPLAY button until the Manual LED lights This will cause the manual display screen to be shown with the previously entered set point temperature 20 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 4 Using Your Stoppering Tray Dryer SET POINT TEMP 30 C The temperature units are displayed in the units F or C selected in the Set Up The temperature may be set anywhere from 40 C to 40 C in 1 C increments 3 If the set point needs to be changed press the INCREASE or DECREASE button until the desired set point temperature is displayed 4 Press ENTER If ENTER is not pressed within 10 seconds the set point will revert to the previously entered set point temperature 5 Press MODE button until the Manual LED lights 6 Press RUN STOP button The amber LED by the button will light and the refrigeration system and or heater will operate 7 To change the set point temperature in the middle
57. T WASHER 4 PLACES STOPPERING TRAY DRYER REMOVE FLAT GASKET IF SO EQUIPPED 114 FLAT WASHER 14 PLACES 1 4 20 KEPS NUT 4 PLACES FREEZE DRYER Product Service Domestic 1 800 522 7658 International 816 333 8811 11 Chapter 3 Getting Started Lift the Stoppering Tray Dryer into place on your Freeze Dry System while fitting the vacuum coupling over the manifold port Align the four mounting holes in the Stoppering Tray Dryer support stand with the four holes in the top of the Freeze Dry System NOTE Do not lift the Stoppering Tray Dryer by the door or disturb it Install the four bolts nuts and washers provided Loosen the clamp and slide it down over the manifold connection port Orient the clamp to gain access and tighten the clamp to provide a leak free connection The Stoppering Tray Dryer is now installed and must be tested to make certain the system is free of leaks To test turn on the Freeze Dry System refrigeration and allow the temperature to reach 40 or lower Close the door of the Tray Dryer and make sure the Stoppering Control is in the LOWER position and the Vac Release control is in the CLOSED position Start the vacuum pump and monitor the vacuum gauge The vacuum on the Freeze Dry System should reach 0 133 mBar within 30 minutes and should achieve an ultimate vacuum of 0 040 mBar or lower within 18 hours If 0 040 mBar cannot be achieved consult the troubleshooting
58. T position Turn on the refrigeration in the Freeze Dryer in the MAN or AUTO mode according to the instructions in this manual If the sample will be prefrozen in the collector chamber the Freeze Dryer must be started in the MAN mode 2 Set the Drying Chamber temperature according to the Set Up instructions in this manual The set temperature should be lower than the eutectic temperature of the sample NOTE The Drying Chamber is NOT refrigerated If the operating temperature is set below ambient the only source cooling the chamber is the sample itself Product Service Domestic 1 800 522 7658 International 816 333 8811 E 31 Chapter 4 Using Your Freeze Dryer 3 Press the switch marked Shell Freezer Vacuum Chamber to actuate the heater 4 Freeze the sample Before the freeze dry process can occur the product to be freeze dried must be in a frozen state This can be done in a separate freezer or in the Freeze Dryer collector chamber 5 Load the samples The Freeze Dryer collector temperature must be 40 C or colder Replace the chamber lid 6 Start primary drying Turn the vacuum control valve on the top of the Freeze Dryer to VACUUM Start the vacuum pump if the Freeze Dryer was started in the MAN mode 7 Start secondary drying After all the free moisture is removed in the primary drying phase the temperature of the chamber may be increased Do this according to the instructions in the Set Up section of this manua
59. a freeze dry system dilution of the sample with more water will help keep the sample frozen For example a 0 2M solution of acetic acid is much easier to freeze dry than a 0 5M solution About This Manual This manual is designed to help you learn how to install use and maintain your Stoppering Tray Dryer Instructions for performing routine maintenance and making minor modifications to your Stoppering Tray Dryer are also included Chapter 1 Introduction provides a brief overview of the freeze dry process explains the organization of the manual and defines the typographical conventions used in the manual 4 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 1 Introduction Chapter 2 Prerequisites explains what you need to do to prepare your site before you install your Stoppering Tray Dryer Electrical requirements are discussed Chapter 3 Getting Started contains the information you need to properly unpack inspect and install your Stoppering Tray Dryer Chapter 4 Using Your Stoppering Tray Dryer discusses the basic operation of your Stoppering Tray Dryer Information on how to load samples and run the Stoppering Tray Dryer is included Chapter 5 Maintaining Your Stoppering Tray Dryer explains how to perform routine maintenance on your Stoppering Tray Dryer Chapter 6 Using the RS 232 Receptacle describes how to connect a computer for monitoring the operation Chapter 7 Troubleshootin
60. a greater tendency to melt particularly when placed in flasks or exposed to room temperature If a sample containing a volatile substance tends to melt when placed on a freeze dry system dilution of the sample with more water will help keep the sample frozen For example a 0 2M solution of acetic acid is much easier to freeze dry than a 0 5M solution About This Manual This manual is designed to help you learn how to install use and maintain your Freeze Dryer Instructions for performing routine maintenance and making minor modifications to your Freeze Dryer are also included Chapter 1 Introduction provides a brief overview of the Freeze Dryer explains the organization of the manual and defines the typographical conventions used in the manual 4 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 1 Introduction Chapter 2 Prerequisites explains what you need to do to prepare your site before you install your Freeze Dryer Electrical requirements are discussed Chapter 3 Getting Started contains the information you need to properly unpack inspect and install your Freeze Dryer Chapter 4 Using Your Freeze Dryer discusses the basic operation of your Freeze Dryer Information on how to attach samples and run the Freeze Dryer is included Chapter 5 Maintaining Your Freeze Dryer explains how to perform routine maintenance on your Freeze Dryer Chapter 6 Using the RS232 Receptacle describes h
61. arm System Temperature Variations Once the system temperature has stabilized for 20 minutes if the manual set point temperature or automatic hold temperature varies more than 2 C as measured by the system temperature sensor the Red Alarm indicator and the word TMP on the display will flash until the end of the run Vacuum Once the system vacuum is low and stabilized at a point where it changes less than 0 020 mBar in 5 minutes if the vacuum changes more than 0 500 mBar the Red Alarm indicator and the word VAC on the display will flash until the end of the run System Temperature Set Point If during a Ramp mode the system temperature stabilizes without reaching the set point temperature the control will enter the next Hold mode The Red Alarm indicator will flash and the program indicator Px on the display will flash until the end of the run Power Failure If a power failure occurs while a run is in progress the Red Alarm indicator and Run Stop Indicator will flash when the power is restored Once power is restored the process will continue as programmed until completion Pressing Run Stop cancels the flashing warning Temperature Probe When the power is turned on the Stoppering Tray Dryer automatically checks the calibration of all four temperature probes If a probe is out of calibration the alarm LED will flash and the display will show 30 Product Service Domestic 1 800 522 7658 International 816
62. check for any visible damage and for improper installation that might cause a vacuum leak Also check that each sample valve is closed or in the vent position Vacuum Pump Ballast Setting Most vacuum pumps are equipped with a gas ballast mechanism The freeze dry process requires high vacuum Therefore it is recommended that the gas ballast be closed during the operation of the Freeze Dry System If the gas ballast is left open for extended periods of operation the oil can be pumped out the exhaust causing the pump to fail Purge Valve The optional purge valve is installed between the Freeze Dryer collection chamber and the vacuum pump When the green LED above the PURGE switch is illuminated the purge valve is closed and the vacuum pump is isolated from the Freeze Dryer collection chamber During Freeze Dryer start up the refrigeration system pulls the collector coil down to temperature While the collector coil cools the purge valve can be closed and the vacuum pump allowed to run This allows the vacuum pump oil to warm which will evaporate and expel condensed solvents from the oil When the collector coil is down to Product Service Domestic 1 800 522 7658 International 816 333 8811 21 Chapter 4 Using Your Freeze Dryer temperature and the freeze dry process is started the warm pump oil is less likely to condense solvent vapors that are not trapped by the collector coil When the Freeze Dryer is operated in the
63. d on options 79600 followed by two digit number based on options T4200 followed by two digit mumber based on options Serial No Various See Individual Declaration Year of Marnufactare 1995 and Subsequent the undersigned hereby declare that the equipewent specified above conforms to the above Directrve s and Standards See individual Declaration of Conformity which will be signed by the importer for your country Signature Full Name Position An individual version of this declaration ia included with your shipping customs documentation Product Service Domestic 1 800 522 7658 International 816 333 8811 CHAPTER 1 INTRODUCTION Congratulations on your purchase of a Labconco FreeZone Stoppering Tray Dryer which is designed for laboratory lyophilization procedures The refrigerant used in the refrigeration system is CFC free so it will not endanger the environment The unit is easy to install and maintain Proper care and maintenance of this product will result in many years of dependable service Freeze Dry Process Freeze drying is an important process in sample preparation and for the preservation and storage of biologicals pharmaceuticals and foods Of the various methods of dehydration freeze drying lyophilization is especially suited for substances that are heat sensitive Other than food processing e g coffee whole dinners freeze drying has been extensively used in the development of pharmac
64. d stoppering system may be removed from the chamber as an assembly for repairs if needed Remove the acrylic door by taking out the two hex socket head screws located on the right hand end of the cross bar Remove the door gasket Carefully pull loose all of the plastic fasteners located around the periphery of the chamber from the chamber Leave the spacer blocks behind the gasket attached to the gasket Place a support in front of the chamber and slide the shelf and stoppering system out approximately 2 inches Loosen the clamp securing the stoppering diaphragm tube located in the lower center at the back of the chamber and remove the tube Slide the assembly out of the chamber and onto the support The assembly is now ready for repairs Whenever possible do not break the fluid system Reverse the removal procedures for installation of the shelf and stoppering system Make sure the fluid inlet and outlet tubes are routed on top of the assembly Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 7 Troubleshooting Filling the Fluid System Fluid Circulation Valve Fluid Reservoir and Cap Electrical Junction Block Flexible Tubing AYN 1 Make sure the Power Switch is in the OFF position 2 Remove the left cover 3 Remove the insulation and both caps from the fluid circulation valve which is located directly behind the fluid reservoir Item 1 4 Attach a flexible t
65. de of the collector chamber and another in the drain port in the bottom 2 Restart the vacuum system and check your vacuum indication Insufficient vacuum indicates a bad pump or a leak in the connections from the pump to the side of the chamber Product Service Domestic 1 800 522 7658 International 816 333 8811 41 Chapter 7 Troubleshooting The following test is used to check the integrity at the Freeze Dry System collection chamber The figure below points out potential areas to locate a leak Collector Chamber Areas for Potential Leaks 42 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 7 Troubleshooting 1 Remove the stopper from the side of the chamber and place a flat gasket and a freeze dry flask over the connection port Freeze Dry Flask 2 Fill the collection chamber with approximately 2 inches of water enough to cover all fittings Replace the collection chamber lid and turn on the vacuum pump Allow the vacuum pump to run for approximately 5 to 10 seconds If the vacuum pump is left on the water will begin to boil and the test will not be effective Look inside the chamber for any bubbling while the pump is running and after you shut the pump off 3 If bubbling is observed around the bulkhead fittings access the bottom of the chamber and remove the insulation Tighten the appropriate fitting by placing a wrench on the fitting inside the chamb
66. e Domestic 1 800 522 7658 International 816 333 8811 Chapter 1 Introduction sample The volume of the freeze dry flask should be two to three times the volume of the sample In order for lyophilization to occur ice must be removed from the frozen sample via sublimation This is accomplished by the collector and the vacuum pump The collector which should be at least 15 to 20 C colder than the eutectic temperature melting temperature of the sample traps vapor as ice Since the vapor pressure at the collector is lower than that of the sample the flow of water vapor is from the sample to the collector Since this vapor diffusion process occurs very slowly under normal atmospheric conditions a good vacuum is essential to maintain an efficient rate In many applications the maintenance of a vacuum of 0 133 mBar or less is recommended The rate of freeze drying is directly proportional to the vapor pressure and the vapor pressure is dependent upon both eutectic temperature and solute concentration of the sample For example a solution of sodium chloride and water would freeze dry at a slower rate than pure water The eutectic temperature of a sodium chloride solution is about 21 C and at this temperature the vapor pressure is about 1 16 that of water at 0 C Although the eutectic temperature is not dependent upon the concentration of sodium chloride the vapor pressure of the water would decrease as the concentration of sodium chlor
67. e Freeze Dryer 230 60 x x 7960047 12 Liter Cascade Freeze Dryer 230 60 x x x Product Service Domestic 1 800 522 7658 International 816 333 8811 11 Chapter 3 Getting Started Catalog Numbers 6 12 and 18 Liter Console Models Teflon Catalog Coated Purge Drying Shell Number Description Volts Hz Chamber Valve Chamber Freezer 7755030 18 Liter Freeze Dryer 230 50 7755031 18 Liter Freeze Dryer 230 50 X 7755032 18 Liter Freeze Dryer 230 50 x 7755034 18 Liter Freeze Dryer 230 50 x x 7755036 18 Liter Freeze Dryer 230 50 x x 7755037 18 Liter Freeze Dryer 230 50 x x x 7755040 18 Liter Freeze Dryer 230 60 7755041 18 Liter Freeze Dryer 230 60 X 7755042 18 Liter Freeze Dryer 230 60 x 7755044 18 Liter Freeze Dryer 230 60 x x 7755046 18 Liter Freeze Dryer 230 60 x x 7755047 18 Liter Freeze Dryer 230 60 x x x Plus the Following Part Component Description 7403400 User s Manual 1336400 Power Cord 115V or 1342100 Power Cord 230V 1291000 Plug 230V models only 7646000 Vacuum Hose 1967600 Hose Clamps 2 7532900 Collector Chamber Lid 7690800 Collector Chamber Lid Gasket 7408300 Drying Chamber Lid if so equipped 7408400 Drying Chamber and Shell Freezer Lid Gasket if so equipped 7403100 Shell Freezer Lid if so equipped 1429900 Stopper with Drying Chamber onl
68. e electrical protection properties of the Stoppering Tray Dryer may be impaired if the Stoppering Tray Dryer is used inappropriately 16 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 4 Using Your Stoppering Tray Dryer Stoppering Tray Dryer Controls The control panel for the Stoppering Tray Dryer is shown with a description about its function 1 Display Displays all necessary programming and operational data Provides prompts to aid in programming 2 Display Selector Changes format of display from monitor to auto to manual to set up screen 3 Display Indicators Amber lamps indicate which display screen is shown 4 Alarm Indicator Red LED indicates that a system alarm has occurred 5 Decrease Switch Used in programming to decrease a parameter set point Product Service Domestic 1 800 522 7658 International 816 333 8811 17 Chapter 4 Using Your Stoppering Tray Dryer Increase Switch Used in programming to increase a parameter set point Enter Switch Used in programming to enter a selected set point into memory Mode Indicator Amber lamp indicates whether the control is set to operate either in the automatic or manual mode Mode Selector Switch Selects the mode of operation either manual or automatic Run Stop Switch Initiates the start or stop of the lyophilization process Run Stop Indicator Amber lamp burns
69. e equipment is thoroughly cleaned after use e Rubber and plastic components that have been exposed to damaging compounds should be removed and flushed with water e The oil in the vacuum pump should be checked often It must be changed if it is cloudy shows particles or is discolored The useful life of vacuum pump oil can be extended if the vacuum pump is operated for an extended period of time after a freeze dry run This allows contaminants to be purged from the hot oil This must be done with the inlet to the pump blocked off to prevent air from free flowing through the pump This is accomplished by closing all sample valves on a clean dry freeze dry system and turning on the vacuum pump If the pump is operated at an elevated vacuum level gt 10mBar oil may be expelled from the pump and damage could occur Another way to extend the life of the vacuum pump is to install an optional secondary trap in the line between the Freeze Dry System and the vacuum pump Contact Labconco for ordering information With prudent maintenance the FreeZone Freeze Dry System will provide years of service Warranty on the affected parts will be voided if maintenance has been obviously neglected If you have questions about using specific compounds in the Freeze Dry System contact Labconco Technical Service at 1 800 821 5525 or 816 333 8811 or e mail labconco labconco com 14 Product Service Domestic 1 800 522 7658 International 816 333 8811
70. e initiated At no time during the primary drying phase should the product temperature be allowed to rise higher than the eutectic temperature 28 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 4 Using Your Stoppering Tray Dryer The ice collecting coil temperature and the vacuum level should be monitored Higher than desired collector coil temperature or vacuum levels will inhibit or ruin the freeze dry process Stoppering The stoppering operation when desired is performed after the freeze dry process is complete To stopper move the Stoppering control toward the RAISE position This action allows the actuator beneath the bottom shelf to inflate causing the bottom shelf to rise The vials on the shelf will then contact the middle shelf causing it to rise and the top shelf will eventually be contacted and rise When all three shelves have raised and made contact with each other stoppers will be pressed into the vials Monitor the stoppering process by looking through the chamber door When all of the vials appear to be stoppered move the Stoppering control to the LOWER position This opens the diaphragm to the vacuum pump which deflates the diaphragm Opening the vacuum release control also deflates the stoppering diaphragm The Stoppering control should be left in the LOWER position when not stoppering Vacuum Break Backfilling To open the chamber door the vacuum must be released
71. e sucked into the collector chamber This is normal 34 Product Service Domestic 1 800 522 7658 International 816 333 8811 CHAPTER 5 MAINTAINING YouR FREEZE DRYER Under normal operation the Freeze Dryer requires little maintenance The following maintenance schedule is recommended As needed 1 Clean up all spills remove liquids from the chamber 2 Clean lid and gasket using soft cloth sponge or chamois and a mild non abrasive soap or detergent 3 Check oil level of the vacuum pump It should be between MIN and MAX If the oil level is less than an inch 25 4 mm above MIN add oil to proper level 4 If oil shows cloudiness particles or discoloration drain the pump and replace with fresh oil 5 Utilization of acids requires immediate cleaning and neutralization after a run or physical damage to the collector chamber and collector coil will result 6 Check the collection chamber for condensed or frozen solvents and dispose of appropriately Completely empty the collector chamber before the next run or before attempting to start the vacuum pump 7 Ifsample valves leak or stems become difficult to turn pull the stem out of the rubber valve body and apply a thin coat of vacuum grease to the stem Reinsert the stem into the valve body Product Service Domestic 1 800 522 7658 35 Chapter 5 Maintaining Your Freeze Dryer Monthly 1 The rubber components on the Freeze Dryer may eventually 2
72. eave the gasket on and turn a large freeze dry flask upside down to cover the connection port 3 Start the freeze dryer and observe the vacuum indication If the vacuum indication is good then the problem is in the drying chamber or manifold and you should return to Section IT Gaskets Tubing Connections Sample Valves Product Service Domestic 1 800 522 7658 International 816 333 8811 45 Chapter 7 Troubleshooting Freeze Dry Flask The following test allows you to check the pump and the connections from the pump to the vacuum tube 1 Place a rubber stopper in the vacuum port in the left side of the collector chamber and another in the drain port in the bottom 2 Restart the vacuum system and check your vacuum indication Insufficient vacuum indicates a bad pump or a leak in the connections from the pump to the side of the chamber Stopper a Collector Coil 46 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 7 Troubleshooting The following test is used to check the collection chamber integrity The figure below points out potential areas to locate a leak Collector Chamber Areas for Potential Leaks 1 Remove the stopper from the side of the chamber and place a freeze dry flask over the connection port 2 Fill the collection chamber with approximately 2 inches of water enough to cover all fittings Replace the collection chamber lid and turn
73. ent on the concentration and exposure duration Some of the major components of the FreeZone Freeze Dry System that are susceptible to degradation are as follows Acids Buffers Solvents a a s z v 5 3 o 8 5 S es SIZE E Ss Ss os amp S gt os D 2 v E o 3 3 amp O 8 amp sa 5 a g a Ss oe S i lt o E o a S o Lg on as Fe a 2 2 E yp 3s E SE S28 2 GE US ee oS ro p Ss D D 9 o 3 q tu Ss q s Ss em gt Component Material lt 1 k 5 O A lt 1 lt 0U U A a Valve Stem Acetal C D D D D Delrin Collector Acrylic D D D D Lid amp Door Hoses Neoprene C D D C C D D D C D Gaskets amp Valve Bodies Flask Top Silicon C D D D D D C D Rubber Chamber amp Stainless C Fittings Steel Product Service Domestic 1 800 522 7658 International 816 333 8811 13 Chapter 3 Getting Started An accessory glass lid is available for the Freeze Dry Systems C Moderate degradation Limited use D Severe degradation infrequent use recommended immediate thorough cleaning required e Most common compounds used in freeze drying processes if allowed to enter the vacuum pump will degrade the oil and cause damage to the vacuum pump e Sugars and proteins typically will have minimal negative effect on any of the materials of construction When using compounds in the Freeze Dryer that are hostile to the materials of construction it is imperative th
74. er and use a second wrench to turn the nut on the bottom of the chamber Be careful not to damage the evaporator coils or the brazed joints to the refrigeration system Once the fitting is tightened perform the test again Should the bubbling still be present loosen the bulkhead fittings and apply vacuum grease to the O rings then reassemble and test Product Service Domestic 1 800 522 7658 International 816 333 8811 43 Chapter 7 Troubleshooting O Ring and Collector Coil Vacuum Grease 4 If bubbling was observed on the chamber surface the chamber must be replaced This type of leak cannot be successfully repaired The leading cause of a chamber surface leak is corrosive residue left in the chamber after use This test verifies that the vacuum leak is in the Stoppering Tray Dryer 1 Remove the Stoppering Tray Dryer 2 Position a flat gasket over the 3 0 inch diameter vacuum port and turn a large freeze dry flask upside down to cover the connection port 3 Start the freeze dryer and observe the vacuum indication If the vacuum indication is good then the problem is in the Stoppering Tray Dryer and you should proceed to Section IV Stoppering Tray Dryer Freeze Dry Flask 44 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 7 Troubleshooting IV Stoppering Tray Dryer e Inspect the door and door gasket e Inspect the coupling between the freeze dryer and the Stopperin
75. erties of the Freeze Dryer may be impaired if the Freeze Dryer is used inappropriately Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 4 Using Your Freeze Dryer Freeze Dryer Controls The control panel for the Freeze Dryer is shown below with a description about its function 1 LCD Display Displays system operating parameters set up parameters and alarm messages 2 Menu Switch This switch is used to change the display from operating system parameters to set up parameters 3 Select Switch Used to select set up parameters 4 Vacuum Switch Used to start or stop the vacuum pump when operating in manual start up mode 5 Vacuum Indicator This green LED indicates that power is being supplied to the vacuum pump receptacle on the back of the Freeze Dryer 6 Manual Refrigeration Switch Used to start only the refrigeration module 7 Manual Operation Indicator When lit the green LED indicates the Freeze Dryer is being controlled manually by the operator The operator must start each function 8 Auto Mode Switch Used to start or stop the refrigeration and the Auto Mode process Product Service Domestic 1 800 522 7658 International 816 333 8811 19 Chapter 4 Using Your Freeze Dryer 10 11 12 13 14 15 16 17 18 19 Auto Mode Indicator When lit the green LED indicates that the Freeze Dryer is in Auto Mode
76. euticals e g antibiotics and preservation of biologicals e g proteins plasma viruses and cell lines The nondestructive nature of this process has been demonstrated by the retention of viability in freeze dried viruses and microorganisms Freeze drying is a process whereby water or other solvent is removed from frozen material by converting the frozen water directly into vapor without the intermediate formation of liquid water The basis for this sublimation process involves the absorption of heat by the frozen sample in order to vaporize the ice the use of a vacuum pump to enhance the removal of water vapor from the surface of the sample the transfer of water vapor to a collector and the removal of heat by the collector in order to condense the water vapor In essence the freeze dry process is a balance between the heat absorbed by the sample to vaporize the Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 1 Introduction 2 Product ice and the heat removed from the collector to convert the water vapor into ice Freeze Dry Rates The efficiency of the freeze drying process is dependent upon the surface area and the thickness of the sample the collector temperature and vacuum obtained the eutectic point and solute concentration of the sample It is important to remember these factors when trying to obtain efficient utilization of your freeze dry system A listing of selected materials and their a
77. everse IEC plug This plug is included with 230V models This will allow the vacuum pump to be plugged into the receptacle on the back panel of the freeze dryer See Appendix D Freeze Dryer Accessories for vacuum pumps available from Labconco Chamber or Manifold Requirements A freeze drying chamber is not included and must be purchased separately These allow samples to be attached to the Freeze Dryer See Appendix D Freeze Dryer Accessories for available chambers and manifolds 8 Product Service Domestic 1 800 522 7658 International 816 333 8811 CHAPTER 3 GETTING STARTED Now that the site for your Freeze Dryer is properly prepared you are ready to unpack inspect install and test your Freeze Dryer Read this chapter to learn how to unpack and move your Freeze Dryer set up your Freeze Dryer connect the electrical supply source to your Freeze Dryer properly exhaust your Freeze Dryer safely use solvents with your Freeze Dryer The FreeZone Freeze Dry System may weigh as much as 330 Ibs 150 kg depending upon the model If you must lift the Freeze Dryer manually use at least two 2 persons and follow safe lifting guidelines Unpacking Your Freeze Dryer Carefully unpack your Freeze Dryer and inspect it for damage that may have occurred in transit If your Freeze Dryer is damaged notify the delivery carrier immediately and retain the entire shipment intact for inspection by the carrier DO NOT RETURN GOODS W
78. followed when defrosting the collector coil l Pull the collector chamber drain hose out from the front panel of the unit and remove the drain plug Place the drain hose in a suitable container to collect the condensate that will be defrosted off the collector coil Press the DEFROST switch on the control panel The green LED above that switch will illuminate Allow unit to operate in this condition until all condensate is defrosted from the collector coil Dispose of the liquid appropriately Lift out the ice plug after it has melted sufficiently to be removed without force Flush the collector chamber with water and wipe chamber dry If rapid defrost is desired pour warm water into the collector chamber covering no more than the bottom 2 coils If excess water is added it can enter the vacuum port and drain into the vacuum pump Product Service Domestic 1 800 522 7658 International 816 333 8811 29 Chapter 4 Using Your Freeze Dryer 6 Press the DEFROST switch the green LED will be off Reinstall the drain hose plug and slide drain hose back into cabinet through the front panel Dispose of the liquid appropriately collector chamber and collector coil will result Utilization of acid requires immediate cleaning and neutralization after defrost or physical damage to the Do not attempt to chip ice from the collector coil as damage may occur to the coil Never attempt to start the vacuum pump when there is liquid in t
79. g The Tray Dryer will store up to five programs numbered 1 through 5 The five programs once programmed will be retained in memory To program a run select the program number that you want to use and enter the parameters as follows Turn the Power switch to the ON position Press the DISPLAY button until the Auto LED lights NOTE Values shown in this example are for reference only The P in the display will flash and the program number that will be run is shown To select different programs press the UP or DOWN key to change program number Programs through 5 When the desired program number is displayed press ENTER The display will show the parameters that were last entered for this program Pl SEG 1 RAMP 00 0 C MN HOLD 34 C TIME 00 0 If any of the parameters are changed the ENTER key must be pressed for the new value to be stored If the ENTER key is not pressed within 10 seconds after the last parameter adjustment the value will return to the previously stored value The flashing parameter name indicates the parameter that will be changed Pressing ENTER only will advance to the next parameter After the AUTO RUN cycle is started segments with a value greater than the segment running may have their parameters changed Only the selected program may be modified To modify a different program the system must be stopped and the desired program selected Starting the Freeze Dry Cycle After the desired c
80. g Tray Dryer e Remove the top left hand cover panel and inspect the valve and hose connections to the chamber e Remove the top right hand cover and inspect the electrical pass through and gasket on the top of the chamber Refrigeration Module Operation Under a no load condition and depending on the ambient temperature the Stoppering Tray Dryer refrigeration system can achieve a system temperature of 40 C or lower within 4 hours when the vacuum pump is running If any repairs are required on the refrigeration module contact your local laboratory supply dealer If your laboratory supply dealer is unable to provide assistance please call Labconco Repairs should only be undertaken by a competent refrigeration technician or through an authorized Labconco service agency Access to Mechanical Components 1 To gain access to the refrigeration system pump tank and the controller and control panel components it is necessary to remove the cover on the left side 2 Remove the stainless steel front panel and control panel Disconnect the wires to the power switch Remove the left cover 3 Additional access is available by removing the remaining screws which hold the rear panel in place and lifting it off the unit Product Service Domestic 1 800 522 7658 International 816 333 8811 45 Chapter 7 Troubleshooting Shelf and Stoppering System Removal 1 2 3 4 5 6 7 The shelf an
81. g contains information about problems you may encounter while using your Stoppering Tray Dryer including the probable causes of the problems and suggested corrective actions Chapter 8 Modifying Your Stoppering Tray Dryer Display describes how to calibrate the vacuum display and restore factory settings Appendix A Stoppering Tray Dryer Components contains labeled diagrams of the components of the Stoppering Tray Dryer Appendix B Stoppering Tray Dryer Dimensions contains comprehensive diagrams showing the dimensions for the Stoppering Tray Dryer Appendix C Stoppering Tray Dryer Specifications contains product specifications A wiring diagram for the Stoppering Tray Dryer is also included Appendix D Stoppering Tray Dryer Accessories lists the part numbers and descriptions of all of the accessories available for your Stoppering Tray Dryer Product Service Domestic 1 800 522 7658 International 816 333 8811 5 Chapter 1 Introduction Typographical Conventions Recognizing the following typographical conventions will help you understand and use this manual e Book chapter and section titles are shown in italic type e g Chapter 3 Getting Started e Steps required to perform a task are presented in a numbered format e Comments located in the margins provide suggestions reminders and references e Critical information is presented in boldface type in paragraphs that are preceded by the exclamation ico
82. he LCD display will show the actual temperature of the collector When the vacuum in the system is above 5 mBar the vacuum display will indicate HI At 5 mBar and below the display will show the actual vacuum When the system vacuum is between 0 450 and 0 133 mBar the lower green vacuum graph LED will flash When the system vacuum level is lt 0 133 mBar the green LED will be lit steadily indicating that samples may be added 26 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 4 Using Your Freeze Dryer Setting the Operating Vacuum Level The vacuum level may be set by the user to optimize the freeze dry process Normally the sublimation rate will increase if there is less vacuum a higher pressure in the Freeze Dryer A good starting place is to set the vacuum so its level is equivalent to about 10 C colder than the eutectic or collapse temperature of the sample Adjustments to the vacuum level must be made for various freeze drying conditions Factors that must be considered are whether the sample is freeze dried on heated shelves or in glassware attached to manifold valves the volatility of the sample itself the size of the sample and the heat energy supplied to the sample When the vacuum control is set to operate at less vacuum the ice holding capacity of the collector may be decreased This can be improved in non cascade models by installing a baffle in the collector See Appendix D Freeze Dr
83. he available receptacle remove this plug and replace it with an approved plug of the suitable style Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 2 Prerequisites Location Requirements The Freeze Dryer should be located in an area that provides an unobstructed flow of air around the cabinet This air cools the refrigeration system The refrigeration system draws air in through the sides and exhausts it through the rear A minimum of 3 must be allowed between the rear and both sides of the Freeze Dryer and adjacent wall surfaces Restriction of airflow during operation could adversely affect performance Refer to Appendix C Freeze Dryer Specifications for dimensional drawings of the Freeze Dryer Vacuum Pump Requirements A vacuum pump must be provided by the user A vacuum pump with a displacement of 144 liters per minute and 0 0002 mBar ultimate pressure is adequate for most samples The inlet fitting on the vacuum pump must be suitable for 3 4 ID vacuum hose which is provided It is recommended that the vacuum pump is equipped with an exhaust filter to minimize oil mist exhausting from the vacuum pump The operating vacuum level may be set on the Freeze Dryer The higher the pressure is set the more likely it is that oil mist will be exhausted Vacuum pumps used with 115V models should be equipped with an 115V 15 Amp NEMA 5 15P plug Vacuum pumps used with 230V models should be equipped with a r
84. he collector chamber This could result in damage to the vacuum pump Operating the Shell Freezer The optional built in shell freezer is designed for shell freezing samples in flasks in preparation for freeze drying Follow the steps below each time you use the shell freezer to obtain optimum performance 1 2 3 6 Check that the solvent bath drain plug is securely installed in the drain hose Remove the bath compartment cover and add solvent to the bath compartment Commonly used solvents are methanol or ethanol Recommended solvent depth is 1 4 to 2 above the top of the rollers approximately 2 liters If flammable solvents are used in the shell freezer bath be sure to keep away from open flame Press the panel switch labeled SHELL FREEZE The green LED above the switch will illuminate The shell freezer refrigeration module will start and the bath rollers will begin rotating The LCD display will show the shell freezer bath temperature Fill a freeze dry container no more than 4 full with sample and stopper the container top Lay the container on the rollers in a horizontal position Replace the bath compartment cover during shell freezing When the sample is completely frozen in the container remove the container from the bath compartment and freeze dry the sample or place it in a suitable storage freezer for future freeze drying Press the SHELL FREEZE switch to turn shell freezer off 30 Product Service
85. he eutectic temperature is not dependent upon the concentration of sodium chloride the vapor pressure of the water would decrease as the concentration of sodium chloride increased This is due to the fact that as the solute concentration increases less of the surface area of the frozen sample is occupied by water In general most solutions or biological samples will have a eutectic temperature of 10 to 25 C However if the sample contains a simple sugar such as glucose or if the sample is animal or plant tissue the eutectic temperature may be as low as 30 to 50 C Freeze Dry Capacity The volume of a sample that can be freeze dried at one time is related to factors discussed previously and the size and design of the freeze dry system With any given instrument the capacity is based on the surface area of the sample the eutectic temperature and concentration of the sample and the rate and amount of heat transferred to the frozen sample Of these factors the eutectic temperature is the most important factor in determining the amount of sample that can be freeze dried at one time particularly when flasks are used This is because as the eutectic temperature decreases the vapor pressure decreases but the rate of heat absorption by the sample does not change This tends to promote melting of the sample which leads to a marked increase in vapor Product Service Domestic 1 800 522 7658 International 816 333 8811 3 Chapter
86. how system temperature system vacuum and 3 sample temperatures if sensors were plugged into their jacks at the front of the chamber and inserted into sample vials If sensors are not plugged into their jacks the probe temperature display will show 26 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 4 Using Your Stoppering Tray Dryer oe The temperatures and vacuum are displayed in the units selected in Set Up Above 5 0 mBar the display will show HI vacuum If the temperature is warmer than 50 C the display will show HI If the temperature is cooler than 50 C the display will say LO Shelf Spacing Adjustment Prior to loading the shelves with the product to be freeze dried adjust the shelves to the 3 shelf 2 shelf or 1 shelf position It is best to observe the shelf supporting mechanism and practice while reading these procedures In the 3 shelf position the spacing between the shelves will accommodate a serum bottle with the stopper raised up to a maximum height of 75 mm 2 9 inches Minimum serum bottle height with lowered stopper for bottles on 3 shelves is 38 mm 1 5 inches For a 2 shelf system grasp the top shelf and raise it until it latches in place Then raise the middle shelf approximately 1 inch until it latches in a position to allow a two equally spaced shelf system The spacing between shelves will accommodate a bottle with the stopper raised up
87. ide increased This is due to the fact that as the solute concentration increases less of the surface area of the frozen sample is occupied by water In general most solutions or biological samples will have a eutectic temperature of 10 to 25 C However if the sample contains a simple sugar such as glucose or if the sample is animal or plant tissue the eutectic temperature may be as low as 30 to 50 C Freeze Dry Capacity The volume of a sample that can be freeze dried at one time is related to factors discussed previously and the size and design of the freeze dry system With any given instrument the capacity is based on the surface area of the sample the eutectic temperature and concentration of the sample and the rate and amount of heat transferred to the frozen sample Of these factors the eutectic temperature is the most important factor in determining the amount of sample that can be freeze dried at one time particularly when flasks are used This is because as the eutectic temperature decreases the vapor pressure decreases but the rate of heat absorption by the sample does not change This tends to promote melting of the sample which leads to a marked increase in vapor Product Service Domestic 1 800 522 7658 International 816 333 8811 3 Chapter 1 Introduction pressure and ultimately overloads the collector and vacuum pump Samples that have eutectic temperatures of 20 C or lower should be placed on the
88. in 18 hours when the refrigeration is operating If the Freeze Dryer does not obtain a satisfactory vacuum perform the following maintenance tests I Vacuum Pump First make sure that the vacuum pump operates If it fails to operate check the electrical connections of the Freeze Dryer to the power source and then check the electrical connection of the vacuum pump to the Freeze Dryer If the vacuum pump has a power switch make sure that it is turned on If the vacuum is not adequate when the vacuum pump is operating proceed with the following steps 1 Check the oil and ensure it is clear and clean If the oil looks cloudy or has any particulates replace the pump oil Sometimes it may be necessary to flush the pump with clean oil several times To flush the pump run the pump 5 to 10 minutes to allow the oil to warm up Drain the oil and refill with clean oil Repeat as necessary 2 Check the oil level in the pump Ensure it is filled to the correct level 3 Check vacuum hose connections from the pump to the Freeze Dryer and try running the unit Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 7 Troubleshooting If vacuum problems continue consider obtaining a second vacuum gauge capable of reading a vacuum of 0 010 mBar It is often useful in determining if the vacuum pump is operating properly and the vacuum sensor reading is accurate 4 Isolate the pump by disconnecting the vacuum hose from
89. l 8 Shut Down After completion of the freeze dry procedure a Press the Shell Freezer Vacuum Chamber Switch to turn off the chamber heater b Release vacuum in the chamber by turning the valve on the top of the Freeze Dryer to VENT Remove the sample d Release vacuum from the Freeze Dryer by either opening the Vacuum Chamber valve when the chamber lid is off or by removing the drain plug or by opening a valve on chamber or manifold mounted on top of the Freeze Dryer Turn off the vacuum pump e Turn off the Freeze Dryer defrost and drain the chamber per instructions in this manual e Alarms A number of unusual events may occur during a lyophilization procedure that can adversely effect the operation of the Freeze Dryer If an event occurs the alarm indicator will flash and the beeper will sound The beeper will automatically mute itself after one minute The specific alarm can be identified by pressing MENU Pressing MENU multiple times will display multiple alarms if they have occurred The following out of specification conditions will initiate an alarm Power Failure If a power failure occurs during a Freeze Dry process the vacuum control valve will allow air to bleed into the Freeze Dryer System 32 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 4 Using Your Freeze Dryer If the failure is of a short duration and the collector does not warm up excessively when power is
90. l Start Up Models not equipped with a purge valve To manually run the freeze dry process press the REFRIGERATION MAN switch This will start the refrigeration system The green LED above the switch will illuminate When the collector temperature reaches 40 C the vacuum pump may be started by pressing the VACUUM switch The Temperature and Vacuum Graphs will indicate collector temperature and system vacuum The LCD display will show the actual temperature of the collector When the vacuum in the system is above 5 mBar the vacuum display will indicate HI At 5 mBar and below the display will show the actual vacuum When the system vacuum is between 0 450 and 0 133 mBar the lower green vacuum graph LED will flash When the system vacuum level is lt 0 133 mBar the green LED will be lit steadily indicating that samples may be added Manual Start Up Models equipped with a purge valve To manually run the Freeze Dryer press the REFRIGERATION MAN switch The green LED above the switch will illuminate The PURGE switch and VACUUM switch may be pressed LED s above the switches will illuminate The purge valve will close and the vacuum pump will start Do not start the vacuum pump without first closing the purge valve When the collector temperature reaches 40 C or any time afterwards press the PURGE switch to open the purge valve The Temperature and Vacuum Graphs will indicate collector temperature and system vacuum T
91. l freezer or the heater on the vacuum chamber if the model is so equipped Shell Freezer Vacuum Chamber Indicator This green LED illuminates when either the shell freezer or vacuum chamber heater is operating 20 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 4 Using Your Freeze Dryer Operation Checklist The following checklist should be followed prior to each use of your Freeze Dryer 1 Wipe the interior of the collector chamber with a soft cloth or paper towel to remove any accumulated moisture 2 Check the collector chamber drain hose to ensure that the hose is free of moisture and that the drain plug is securely installed The Freeze Dryer will not start if moisture is detected 3 Using a soft lint free cloth or paper towel wipe the collector chamber lid gasket to remove any dirt and contaminants that could cause a vacuum leak Vacuum grease is not required on the lid gasket to obtain a proper vacuum seal 4 Remove the accessory drying chamber or manifold from the connection port and using a soft lint free cloth or paper towel wipe the port gasket and sealing surfaces of the drying chamber manifold to remove any dirt and contaminants that could cause a vacuum leak Reinstall the drying chamber or manifold on the port Vacuum grease is not required on the port gasket to obtain a proper vacuum seal 5 Inspect each sample valve on the accessory drying chamber or manifold and
92. let This outlet requires a 20 Amp circuit breaker or fuse for models rated at 115V 60 Hz An outlet equipped with a 15 Amp circuit breaker or fuse is required for models rated at 230V 50 60 Hz The power cord on 115V models is equipped with a 20 Amp NEMA 5 20P plug The power cord on 230V models is equipped with a NEMA 6 20P plug If this does not match with the Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 2 Prerequisites available receptacle remove this plug and replace it with an approved plug of the suitable style Location Requirements The Freeze Dryer should be located in an area that provides an unobstructed flow of air around the cabinet This air cools the refrigeration system The refrigeration system draws air in through the front and exhausts it through the rear A minimum of 3 must be allowed between the rear and both sides of the Freeze Dryer and adjacent wall surfaces Restriction of airflow during operation could adversely affect performance Refer to Appendix B Stoppering Tray Dryer Dimensions for dimensional drawings of the Stoppering Tray Dryer Vacuum Pump Requirements A vacuum pump must be provided by the user A vacuum pump with a displacement of 144 liters per minute and 0 0002 mBar ultimate pressure is adequate for most samples The inlet fitting on the vacuum pump must be suitable for 3 4 ID vacuum hose which is provided with the FreeZone Freeze Dry System It is reco
93. ly a few milliliters However for larger volumes the samples should be shell frozen to maximize the surface area and minimize the thickness of the 2 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 1 Introduction sample The volume of the freeze dry flask should be two to three times the volume of the sample In order for lyophilization to occur ice must be removed from the frozen sample via sublimation This is accomplished by the collector and the vacuum pump The collector which should be at least 15 to 20 C colder than the eutectic temperature melting temperature of the sample traps vapor as ice Since the vapor pressure at the collector is lower than that of the sample the flow of water vapor is from the sample to the collector Since this vapor diffusion process occurs very slowly under normal atmospheric conditions a good vacuum is essential to maintain an efficient rate In many applications the maintenance of a vacuum of 0 133 mBar or less is recommended The rate of freeze drying is directly proportional to the vapor pressure and the vapor pressure is dependent upon both eutectic temperature and solute concentration of the sample For example a solution of sodium chloride and water would freeze dry at a slower rate than pure water The eutectic temperature of a sodium chloride solution is about 21 C and at this temperature the vapor pressure is about 1 16 that of water at 0 C Although t
94. m tubing for signs of deterioration or cracking Check all connections and make sure they are secure and leak tight Check the Freeze Dry System collector lid gasket and the Stoppering Tray Dryer door gasket for indentations cracks or tears Clean gaskets using a soft lint free cloth or paper towel The Stoppering Tray Dryer chamber and base unit collector chamber must be dry When checking the sample valves if the system is so equipped pull as much vacuum as possible If a vacuum indication is displayed wiggle or rotate the valves and watch the gauge for any fluctuations Fluctuations can indicate a potential vacuum leak If the valve seems to be in good condition remove the valve and apply a thin coat of vacuum grease to the stem and the outside sealing surface of the valve body and reinstall the valve If the valve still seems to be the source of the problem remove the valve and stopper the hole with a rubber stopper Continue checking the other valves 40 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 7 Troubleshooting The illustration below shows how the sample valve installs on a manifold Manifold Assembly Knob amp Stem Valve Body Trim Ring Assembly System Components and Collection Chamber Isolation The following test allows you to check the pump and the connections from the pump to the vacuum tube 1 Place a rubber stopper in the vacuum port in the left si
95. mmended that the vacuum pump is equipped with an exhaust filter to minimize oil mist exhausting from the vacuum pump The operating vacuum level may be set on the Freeze Dry System The higher the pressure is set the more likely it is that oil mist will be exhausted Vacuum pumps used with 115V models should be equipped with an 115V 15 Amp NEMA 5 15P plug Vacuum pumps used with 230V models should be equipped with a reverse IEC plug This plug is included with 230V models This will allow the vacuum pump to be plugged into the receptacle on the back panel of the Freeze Dry System Refer to the User s Manual for the FreeZone Freeze Dry System for vacuum pumps available from Labconco 8 Product Service Domestic 1 800 522 7658 International 816 333 8811 CHAPTER 3 GETTING STARTED Now that the site for your Stoppering Tray Dryer is properly prepared you are ready to unpack inspect install and test your Stoppering Tray Dryer Read this chapter to learn how to e unpack and move your Stoppering Tray Dryer e setup your Stoppering Tray Dryer e connect the electrical supply source to your Stoppering Tray Dryer e safely use solvents with your Stoppering Tray Dryer The Stoppering Tray Dryer weighs over 400 Ibs 181 Kg The carton allows for lifting with a mechanical lift truck or hand truck If you must lift the Stoppering Tray Dryer manually use at least four 4 persons and follow safe lifting guidelines Unpacking Your Stop
96. mplete Lyph Lock Flask includes e a flask top of high strength borosilicate glass e a flexible non contaminating silicone rubber seal e a flask bottom of borosilicate glass to with stand extreme temperatures and high vacuum Available in seven convenient sizes Entire flask may Compatible with all major brands of labo ratory freeze dry apparatus Silicone rubber seal grasps top and bottom The flexible ring holds securely together during pre freezing and lyophiliza tion Flat bottom reduces spills provides better be autoclaved balance Provides a high vacuum seal for efficient lyophilization Adapters Add the Adapters for connecting the Lyph Lock Flasks to the valve ports on your drying chamber or manifold iss PepPYW Dl 7 90 Bend Description Adapter 7568000 Connects 19 38 ST Flask Top to 1 2 valve 7568200 Connects 19 38 ST Flask Top to 3 4 valve 7568400 Connects 24 40 STJ Flask Top to 1 2 valve 7568600 Connects 24 40 ST Flask Top to 3 4 valve EEE E Valves on the freeze dry systems drying chambers and manifolds offered in this catalog fit adapters of both 1 2 and 3 4 sizes Size information is provided for selecting adapters for older Labconco models and other freeze dryers Product Service Domestic 1 800 522 7658 International 816 333 8811 73 Appendix D Freeze Dryer Accessories Serum Bottles and Vials Pe
97. n Failure to comply with the information following an exclamation icon may result in injury to the user or permanent damage to your Freeze Dryer e Important information is presented in capitalized type in 185 paragraphs that are preceded by the pointer icon It is imperative that the information contained in these paragraphs be thoroughly read and understood by the user 6 Product Service Domestic 1 800 522 7658 International 816 333 8811 CHAPTER 2 PREREQUISITES Before you install your Stoppering Tray Dryer you need to prepare your site for installation The Stoppering Tray Dryer will mount on top of a FreeZone 6 12 or 18 liter Freeze Dry System This could be either a benchtop or console model Carefully examine the location where you intend to install your Stoppering Tray Dryer You must be certain that the area is level and of solid construction An electrical source must be located near the installation site Carefully read this chapter to learn e the electrical supply requirements e the vacuum pump requirements Refer to Appendix C Stoppering Tray Dryer Specifications for complete Stoppering Tray Dryer electrical and environmental conditions specifications and requirements Refer to the User s Manual for the FreeZone Freeze Dry System for complete electrical and environmental conditions specifications and requirements Electrical Requirements The Stoppering Tray Dryer requires a dedicated electrical out
98. n Manual Mode The display will default to the main freeze dry display information If you do not want to restore all factory settings but want to adjust offsets press MENU briefly and the display will show COLLECTOR TEMP OFFSET O Q Press SELECT until the appropriate offset is shown Each number represents 1 C Press MENU and if the drying chamber has been installed the display will show SDC TEMP OFFSET OC Press SELECT until the appropriate offset is shown Each number represents 1 C Press MENU and the display will show VACUUM OFFSET O uBar Press SELECT until the appropriate offset is shown Each number represents 0 001 mBar Press MENU and the display will show LOW LINE OFFSET Press SELECT until the appropriate offset is shown If the Freeze Dryer is operating on nominal 115V each number represents 2V If3 is entered into the display the low line alarm will alarm when the voltage drops to approximately 97V for example 103 2x3 97V Ifthe Freeze Dryer is operating on nominal 230V each number represents 4V if 3 is entered into the display the low line alarm will alarm when the voltage drops to approximately 194V for example 206 4x3 194V There will be no alarm indicated if DISABLED is selected Product Service Domestic 1 800 522 7658 International 816 333 8811 51 Chapter 8 Modifying Your Freeze Dryer Display Press MENU and the display will show HIGH LINE OFFSET 0 Pre
99. o flush the pump run the pump 5 to 10 minutes to allow the oil to warm up Drain the oil and refill with clean oil Repeat as necessary 2 Check the oil level in the pump Ensure it is filled to the correct level 3 Check vacuum hose connections from the pump to the Freeze Dryer and try running the unit Product Service Domestic 1 800 522 7658 International 816 333 8811 39 Chapter 7 Troubleshooting If vacuum problems continue consider obtaining a second vacuum gauge capable of reading a vacuum of 0 010 mBar It is often useful in determining if the vacuum pump is operating properly and the vacuum sensor reading is accurate 4 Isolate the pump by disconnecting the vacuum hose from the Freeze Dry System Deadhead the pump by inserting the vacuum sensor from a secondary vacuum gauge into the end of the vacuum hose and observe the vacuum reading obtained Confirm that the pump is capable of achieving an ultimate vacuum less than 0 010 mBar or approximately 10 microns If an inadequate vacuum reading is obtained the pump has most likely failed and may need to be replaced or rebuilt ll Gaskets Tubing Connections Sample Valves 1 Check all sample valves on the optional 6 port manifold shelf if it is installed and ensure all valves are closed or in the vent position Check the drain line on the Freeze Dry System and ensure the drain plug is installed and the tube appears to be in good condition Check all rubber vacuu
100. oduct Service Domestic 1 800 522 7658 International 816 333 8811 Appendix D Stoppering Tray Dryer Accessories Serum Bottles amp Vials Product Service Domestic 1 800 522 7658 International 816 333 8811 61 DECLARATION OF CONFORMITY Application Council Directive s 73 23 EEC 89 336 EEC Standard s to which conformity is declared EN61010 EN55014 EN55104 Manufacturer s Name Labconco Corporation Manufacturer s Address 8811 Prospect Avenue Kansas City MO 64132 USA Importer s Name See Shipping Customs Documents Importer s Address See Shipping Customs Documents for your equipment Type of Equipment Laboratory Equipment Sample Preparation Model No Stoppering Tray Dryer 230V 7948030 Serial No Various See Individual Declaration Year of Manufacture 2004 and Subsequent I the undersigned hereby declare that the equipment specified above conforms to the above Directive s and Standard s See individual Declaration of Conformity which will be signed by the importer for your country Signature Full Name Position An individual version of this declaration is included with your shipping customs documentation Labconco P N 36960 10 REV B ECO C484 Product Service Domestic 1 800 522 7658 International 816 333 8811
101. of a run repeat steps 2 3 and 4 The system will adjust to the new temperature set point 8 To monitor system operation press DISPLAY until the Monitor LED lights The display will simultaneously show system temperature vacuum and three sample temperatures if sensors were plugged into their jacks at the front of the chamber and inserted into sample vials If sensors are not plugged into their jacks the probe temperature display will show The segment number will always indicate M while operating in the manual mode Segment numbers are used only in the automatic mode to identify portions of the programmed cycle Temperatures and vacuum are displayed in the units selected during the set up procedure Above 5 0 mBar the display will show hi vacuum System temperature rather than probe temperature is the parameter that is regulated by the controller Product Service Domestic 1 800 522 7658 International 816 333 8811 21 Chapter 4 Using Your Stoppering Tray Dryer Pl indicates what program is selected PRB shelf probes for shelf 1 2 and 3 If a probe is not installed the display shows C C P1 PRB 1 XX 2 XX 3 XXc TMP XX SEG M VAC hi m F F TMP system temperature SEG indicates what segment is active and ramping or holding M manual mode VAC system vacuum level m mBar P Pascal T Torr R Ramp H Hold TR Time remaining in hours 9 To stop push RUN STOP butt
102. on which will turn off the amber LED over the switch the refrigeration system and the heater To turn off the entire system turn the power switch off Automatic Control Operation The Stoppering Tray Dryer is equipped with a microprocessor based controller that permits temperature to be programmed using as many as five different segments Each segment consists of a temperature ramp function and a temperature hold function There are five programs of five segments each that store the settings One of the five may be selected by pressing the DISPLAY switch until the AUTO LED lights Press the UP DOWN keys to select the desired program and then press ENTER The display will change to show the parameters for this program The ramp allows the temperature of the sample to be increased or decreased at any desired rate within the capacity of the heating and cooling systems of the Stoppering Tray Dryer A Stoppering Tray Dryer without samples on shelves is capable of cooling at a rate of approximately 5 C minute and can heat at approximately 1 3 C minute The cooling ramp rate may be slower as the temperature approaches 40 C Hold temperatures may be set anywhere from 40 C to 40 C in 1 C increments When the desired temperature is achieved the hold function will maintain that temperature for the programmed length of time The microprocessor control has a built in memory of the last entered 22 Product Service Domestic 1 800
103. on the vacuum pump Allow the vacuum pump to run for approximately 5 to 10 seconds If the vacuum pump is left on the water will begin to boil and the test will not be effective Look inside the chamber for any bubbling while the pump is running and after you shut the pump off 3 If bubbling is observed around the bulkhead fittings access the bottom of the chamber and remove the insulation Tighten the appropriate fitting by placing a wrench on the fitting inside the chamber and use a second wrench to turn the nut on the bottom of the chamber Be careful not to damage the evaporator coils or the brazed joints to the refrigeration system Once the fitting is tightened perform the test again Should the bubbling still be present loosen the bulkhead fittings and apply vacuum grease to the O rings then reassemble and test Product Service Domestic 1 800 522 7658 International 816 333 8811 47 Chapter 7 Troubleshooting COLLECTOR COL 1 O Ring and Vacuum Grease Collector Coil 4 If bubbling was observed on the chamber surface the chamber must be replaced This type of leak cannot be successfully repaired The leading cause of a chamber surface leak is corrosive residue left in the chamber after use Refrigeration Module Operation Under a no load condition the FreeZone Single Stage Freeze Dry System can achieve a collector temperature of 50 C or lower when the system is under vacuum within 40 minutes when the
104. ored by looking through the chamber door Cease stoppering when all bottles appear stoppered or if a problem occurs Distributing the serum bottles evenly on the shelves also aids in consistent drying of all serum bottles on each shelf Sample Freezing Before the freeze dry process can occur the products to be dried must be in a frozen state This can be accomplished in a freezer separate from the Stoppering Tray Dryer or on the shelves in the Stoppering Tray Dryer First the shelves should be adjusted to accept the size of the selected sample containers Next turn On the power switch and set the controls to cool the shelves This is most simply done by setting the temperature in the manual mode although segment 1 in the automatic mode can also be programmed to cool the shelves and start the vacuum after the end of Segment 1 Load the samples onto the shelves after the system temperature is below the sample eutectic temperature If desired place one temperature probe in a sample vial on each shelf The temperature can be monitored by pressing the Display button until the Monitor LED lights Freeze Drying Turn on the FreeZone Freeze Dry System base unit Following the instructions for the unit this may be accomplished in either the automatic or manual mode When the collector temperature is less than 40 C and the vacuum is less than 0 133 mBar the manual mode set point temperature may be adjusted or the automatic mode program may b
105. ow to connect a computer for monitoring the operation Chapter 7 Troubleshooting contains a table of problems you may encounter while using your Freeze Dryer including the probable causes of the problems and suggested corrective actions Chapter 8 Modifying Your Freeze Dryer Display describes how to calibrate the vacuum display restore factory settings Appendix A Freeze Dryer Components contains labeled diagrams of the components of the Freeze Dryer Appendix B Freeze Dryer Dimensions contains comprehensive diagrams showing the dimensions for the Freeze Dryer Appendix C Freeze Dryer Specifications contains product specifications A wiring diagram for the Freeze Dryer is also included Appendix D Freeze Dryer Accessories lists the part numbers and descriptions of all of the accessories available for your Freeze Dryer Product Service Domestic 1 800 522 7658 International 816 333 8811 5 Chapter 1 Introduction Typographical Conventions Recognizing the following typographical conventions will help you understand and use this manual e Book chapter and section titles are shown in italic type e g Chapter 3 Getting Started e Steps required to perform a task are presented in a numbered format e Comments located in the margins provide suggestions reminders and references e Critical information is presented in boldface type in paragraphs that are preceded by the exclamation icon Failure to comply
106. p bit 4 No parity is transmitted 5 Standard ASCII character set 34 Product Service Domestic 1 800 522 7658 International 816 333 Chapter 6 Using the RS232 Receptacle The time between data transmissions may be varied by the user to occur at 10 30 60 300 or 600 second intervals Press the MENU button on the Freeze Dryer base unit until the RS232 screen appears on the display RS 232 TRANSMISSION RATE 10 SECONDS Press select until the desired time interval is shown The format of the transmitted message with typical values is as follows B lt T 48 V 18 SF 41 C 999 PG 1 gt TD lt PR 1S 3R TR 5678 ST 40 P1 39 P2 999 P3 37 V 0537 gt Where B Base Unit T Collector Temperature 48 Collector Temperature in Celsius V Vacuum 18 Vacuum Level in Micro Bars SF Shell Freezer Temperature if so equipped 41 Shell Freezer Temperature in C C Vacuum Chamber Temperature if so equipped 9 Feature not installed or out of range PG Purge if so equipped 1 ON 0 OFF TD Tray Dryer PR Program 1 Program 1 is selected S Segment 3 Segment 3 is operating R Segment is in Ramp Mode H Segment is in Hold Mode TR Time Remaining of the current Hold Segment 5678 Time Remaining in Hours ST System Temperature 40 System Temperature in C P1 Probe 1 Temperature 39 Probe 1 Temperature in C P2 Probe 2 Temperature 999 Probe not connected or temperature is out of
107. perage w o Max with Catalog Operating Vacuum Vacuum Number Description Nominal Range Frequency Phase Pump Pump 7753042 6 Liter Freeze Dryer 230 187 253 60 1 3 8 7753044 6 Liter Freeze Dryer 230 187 253 60 1 3 8 7753046 6 Liter Freeze Dryer 230 187 253 60 1 3 8 7753047 6 Liter Freeze Dryer 230 187 253 60 1 3 8 7753522 6 Liter Freeze Dryer 115 103 127 60 1 13 16 100 90 110 50 1 13 16 7753524 6 Liter Freeze Dryer 115 103 127 60 1 13 16 100 90 110 50 1 13 16 7753532 6 Liter Freeze Dryer 230 198 254 50 1 5 5 10 7753534 6 Liter Freeze Dryer 230 198 254 50 1 5 5 10 7753542 6 Liter Freeze Dryer 230 187 253 60 1 5 5 10 7753544 6 Liter Freeze Dryer 230 187 253 60 1 5 5 10 7934020 6 Liter Cascade Freeze Dryer 115 103 127 60 1 11 16 100 90 110 50 1 11 16 7934021 6 Liter Cascade Freeze Dryer 115 103 127 60 1 11 16 100 90 110 50 1 11 16 7934022 6 Liter Cascade Freeze Dryer 115 103 127 60 1 11 16 100 90 110 50 1 11 16 7934024 6 Liter Cascade Freeze Dryer 115 103 127 60 1 11 16 100 90 110 50 1 11 16 7934026 6 Liter Cascade Freeze Dryer 115 103 127 60 1 11 16 100 90 110 50 1 11 16 7934027 6 Liter Cascade Freeze Dryer 115 103 127 60 1 11 16 100 90 110 50 1 11 16 7934030 6 Liter Cascade Freeze Dryer 230 198 254 50 1 5 5 10 7934031 6 Liter Cascade Freeze Dryer 230 198 254 50 1 5 5 10 7934032 6 Liter Cascade Freeze Dryer 230 198 254 50 1 5 5 10 7934034 6 Liter Cascade Freeze Dryer 230 198 254 50 1 5 5 10 7934036 6 Liter Cascade Freeze Dryer 230 198 254 50 1 5 5 10
108. pering Tray Dryer Carefully unpack your Stoppering Tray Dryer and inspect it for The United States damage that may have occurred in transit If your Stoppering Tray Interstate Commerce Dryer is damaged notify the delivery carrier immediately and Commission rules require that claims be filed with the delivery carrier within fifteen 15 DO NOT RETURN GOODS WITHOUT THE se NE PRIOR AUTHORIZATION OF LABCONCO Product Service Domestic 1 800 522 7658 International 816 333 8811 9 retain the entire shipment intact for inspection by the carrier Chapter 3 Getting Started UNAUTHORIZED RETURNS WILL NOT BE ACCEPTED IF YOUR STOPPERING TRAY DRYER WAS pa DAMAGED IN TRANSIT YOU MUST FILE A CLAIM DIRECTLY WITH THE FREIGHT CARRIER LABCONCO CORPORATION AND ITS DEALERS ARE NOT RESPONSIBLE FOR SHIPPING DAMAGE DO NOT DISCARD THE CARTON OR PACKING MATERIAL FOR YOUR STOPPERING TRAY DRYER UNTIL YOU HAVE CHECKED ALL OF THE COMPONENTS AND INSTALLED AND TESTED THE STOPPERING TRAY DRYER Stoppering Tray Dryer Components Locate the model of Stoppering Tray Dryer you received in the following table Verify that the components listed are present and undamaged Catalog Product Description 7948020 Stoppering Tray Dryer 115V 60 Hz 7948030 Stoppering Tray Dryer 230V 50 Hz 7948040 Stoppering Tray Dryer 230V 60 Hz Plus the following Part Qty Component Description 7353900 1 User s Manual 1336400 1 Power Cord
109. pproximate drying times are shown in Table 1 for your reference Table 1 SAFE TEMPERATURE AND DRYING TIMES FOR SELECTED MATERIALS Material Safe Collector Hours 10mm Thick Temperature Temperature Approx C C Milk 5 40 10 Urea 7 40 10 Blood Plasma 10 to 25 40 16 Serum 25 40 18 Vaccinia 30 to 40 50 22 Influenza Vaccine 30 50 24 Human Tissue 30 to 40 50 48 Vegetable Tissue 50 80 60 Total sample quantities are contingent on various freeze dryer capacities Up to the point of overloading the system the greater the surface area of the sample the faster the rate of freeze drying By contrast for a given surface area the thicker the sample the slower the rate of freeze drying This is based on the fact that the heat of sublimation is usually absorbed on one side of the frozen sample and must travel through the frozen layer to vaporize water at the other surface In addition as the sample is freeze dried the water vapor must travel through the layer of dried material The thicker the sample the greater the chance that the dried layer may collapse which would cause an additional decrease in the rate of freeze drying The surface area and thickness of the sample can usually be ignored when each sample contains only a few milliliters However for larger volumes the samples should be shell frozen to maximize the surface area and minimize the thickness of the Servic
110. r 7522900 7444000 and 7867000 Provides 3 heated shelves operating at 43 C 110 F 115V 7509301 Product Heater For use in chamber 7522900 7444000 and 7867000 Provides 3 heated shelves operating at 43 C 110 F 230V 7509400 Product Heater with Variable Heat For use in chamber 7522900 7444000 and 7867000 Provides variable heat up to 43 C 110 F 115V 7509401 Product Heater with Variable Heat For use in chamber 7522900 7444000 and 7867000 7806020 Bulk Tray Dryer 115V 60 Hz three shelves 630 square inches of area provides heat control 7806021 Bulk Tray Dryer 115V 60 Hz three shelves 630 square inches of area provides heat control with 6 port manifold 7806022 Bulk Tray Dryer 115V 60 Hz three shelves 630 square inches of area provides heat control with RS232 output connection 70 Product Service Domestic 1 800 522 7658 International 816 333 8811 Appendix D Freeze Dryer Accessories PART DESCRIPTION 7806023 Bulk Tray Dryer 115V 60 Hz three shelves 630 square inches of area provides heat control with 6 port manifold and RS232 output connection 7806030 Bulk Tray Dryer 230V 50 60 Hz Three shelves 630 square inches of area provides heat control 7806031 Bulk Tray Dryer 230V 50 60 Hz Three shelves 630 square inches of area provides heat control With 6 port manifold 7806032 Bulk Tray Dryer 230V 50 60 Hz Three shelves 630 square
111. r Temperature 48 Collector Temperature in Celsius V Vacuum 18 Vacuum Level in Micro Bars SF Shell Freezer Temperature if so equipped 9 Feature not installed or out of range C Vacuum Chamber Temperature if so equipped PG Purge if so equipped 1 On 0 Off If a Stoppering Tray Dryer is attached to the Freeze Dryer and the data interconnect cable is installed additional data about that accessory will be transmitted from the Freeze Dryer See the User s Manual for the Stoppering Tray Dryer for a description of the data There are several commercially available software packages which can read RS232 data and enter the data into a computer program such as a word processor to create a text file or 38 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 6 Using the RS232 Receptacle spreadsheet to tabulate and plot the data Consult your laboratory supply dealer regarding the latest software available The following describes how to use an IBM compatible computer with Hyper Terminal software included with Windows 95 98 XP or 2000 operating systems to collect the RS232 data from your Freeze Dryer 1 Make sure that the Freeze Dryer is properly connected to the communication port on the computer 2 Open Hyper Terminal software 1 Windows 95 or 98 use START PROGRAMS ACCESSORIES 11 Windows 2000 or XP use START PROGRAMS ACCESSORIES COMMUNICATIONS
112. r of the Freeze Dry System with a soft cloth or paper towel to remove any accumulated moisture 3 Check the collector chamber drain hose on the Freeze Dry System to ensure that the hose is free of moisture and that the drain plug is securely installed 4 Using a soft lint free cloth or paper towel wipe the Freeze Dry System collector chamber lid gasket and the Stoppering Tray Dryer door gasket to remove any dirt and contaminants that could cause a vacuum leak Vacuum grease is not required on the door gasket or collector lid gasket to obtain a proper vacuum seal Operating the Stoppering Tray Dryer Set Up The display units for vacuum may be selected to be mBar Pascal Pa or Torr and the temperatures may be displayed as either F or C The refrigeration operating time may be monitored and the vacuum reading may be calibrated To configure your Stoppering Tray Dryer turn the main power switch ON Press the Display button until the Set up LED is lit The display will show TEMPERATURE UNITS C es Product Service Domestic 1 800 522 7658 International 816 333 8811 19 Chapter 4 Using Your Stoppering Tray Dryer Press tt or amp until the desired units are flashing Press ENTER The display will show VACUUM UNITS MBar Pa Press tt or until the desired units are flashing Press ENTER The display will show REFRIG TOTAL HOUR XXXX SERVICE HOUR XXXX e Press ENTER if you do not want to reset
113. r stainless steel adapters in 1 2 and 3 4 diameters Diameter Borosilicate Glass 1 2 flask top to 1 2 valve 3 4 flask top to 3 4 valve 1 2 flask top to 3 4 valve 3 4 flask top to 1 2 valve Stainless Steel 1 2 flask top to 1 2 valve 3 4 flask top to 3 4 valve Straight Adapter 7545000 7545200 7545400 7545400 7547000 7547200 45 Bend Adapter 7545600 7545800 7546000 7546000 7547400 7547600 7544810 Replacement Filter Paper 1000 10 packages of 100 1 diameter 28mm Pore size 17 microns Shipping weight 0 5 Ib Compatible with all major brands of laboratory freeze dry apparatus No complex filter retainer is necessary For those who use filters they are easily inserted between the adapter and top of the flask One hun dred filters are sup plied with each flask Wide mouth opening loads fast cleans easily Horizontal shell freezing Flask may be placed in a horizontal posi tion and rotated in a bath for shell freezing Available in nine convenient sizes Flat bottom reduces spills provides better balance 72 Product Service Domestic 1 800 522 7658 International 816 333 8811 Lyph Lock Flasks Lyph Lock Flasks simplify your lyophilization procedures because they have only three pieces per flask a high strength borosilicate glass top and bottom with a silicone rubber ring seal The unique wide mouth design
114. range P3 Probe 3 Temperature 37 Probe 3 Temperature in C V Vacuum at Stoppering Tray Dryer 537 Vacuum in Micro Bars Product Service Domestic 1 800 522 7658 International 816 333 8811 35 Chapter 6 Using the RS232 Receptacle There are several commercially available software packages which can read RS232 data and enter the data into a computer program such as a word processor to create a text file or spreadsheet to tabulate and plot the data Consult your laboratory supply dealer regarding the latest software available The following describes how to use an IBM compatible computer with Hyper Terminal software included with Windows 95 98 XP or 2000 operating systems to collect the RS232 data from your Freeze Dryer 1 Make sure that the Freeze Dryer is properly connected to the communication port on the computer 2 Open Hyper Terminal software 1 Windows 95 or 98 use START PROGRAMS ACCESSORIES 11 Windows 2000 or XP use START PROGRAMS ACCESSORIES COMMUNICATIONS The first time Hyper Terminal is opened a dialogue box requesting an area code and phone number will appear Enter the appropriate numbers and continue 3 The Connection Description dialogue box will open Type in a user defined name and select an icon for the new connection Press OK 36 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 6 Using the RS232 Receptacle
115. restored the Freeze Dryer will restart and resume operation of the refrigeration and vacuum systems If the power failure lasts for a longer duration and the collector warms above safe limits when the power is restored the Freeze Dryer will not restart by itself This prevents melted sample from being drawn into the collector and prevents liquid from being sucked into the vacuum pump When power is restored the alarm indicator will flash and the alarm beeper will sound When the MENU button is pressed the display will show POWER FAIL HOLD SELECT TO CLEAR IT Press and hold SELECT for five seconds until the error message is cleared from the display Line Voltage Out of Range If the voltage supplied to the Freeze Dryer varies beyond allowable limits the alarm will be activated When an alarm occurs press MENU and the display will show LINE VOLTAGE ERROR The alarm will self cancel when the proper voltage is restored The high and low alarm points are preset at the factory to correspond to the normal allowable voltage variations based on the nominal voltage specified for the freeze dryer Some models may be operated outside the normal voltage limits See Appendix C If necessary the high and low alarm points may be adjusted for these models See Chapter 8 Temperature Out of Range An alarm will be activated if the collector temperature rises above 40 C If this occurs the display will show COLLECTOR TEMPERATURE HOL
116. rfect for long term storage of freeze dried samples Labconco Serum Bottles and Threaded Vials are specifically designed for lyophilization applications Their uniform thin wall construction ensures even freezing and drying Bottles and vials are ideal containers for use in the FreeZone Stoppering Tray Dryer Serum bottles also connect to valve ports on drying chambers and manifolds Serum Bottles Serum Bottles Stoppers and Seals are supplied in pack ages of 100 s SS Cc IH GO RSS Size 20 mm 13 mm Split Aluminum Sleeve Type Corkage Corkage Stoppers Seals Stoppers 2ml 7575010 7576010 7577010 3 ml 7575210 7576010 7577010 5 ml 7573010 7576210 7577110 7577510 10 ml 7573210 7576210 7577110 7577510 20 ml 7573410 7576210 7577110 7577510 30 ml 7573610 7576210 7577110 7577510 50 ml 7573810 7576210 7577110 7577510 100 ml 7574010 7576210 7577110 7577510 125 ml 7574210 7576210 7577110 7577510 Threaded Vials Stoppers and Threaded Vials with Screw Caps are supplied in packages of 200 Size Vials with Stoppers Screw Caps 5 ml 7762300 7762200 10 ml 7762600 7762200 9 e em Accessories Seal Crimper Secures tear away Aluminum Seals 7578000 Seal Crimper for 13 mm corkage Shipping weight 3 lbs 1 4 kg 7578100 Seal Crimper for 20 mm corkage Shipping weight 3 lbs 1 4 kg Vacuum Stoppering Adapter 7593000 Adapter connects to valve ports for manual stop pering of 20 mm corkage
117. rying biological substances it may be necessary to decontaminate the system A surface decontaminant should be used to clean the accessible surfaces The use of ethylene oxide is not recommended because of its hazardous and corrosive nature Contact Labconco for additional information Product Service Domestic 1 800 522 7658 International 816 333 8811 33 CHAPTER 6 Usina THe RS232 RECEPTACLE The operation of the Stoppering Tray Dryer and the FreeZone Freeze Dry System can be monitored using a computer when the Stoppering Tray Dryer is connected to the RS232 receptacle on the rear panel of the Freeze Dry System base unit The computer cannot control the operation of the Freeze Dry System Computer Connection for Computer Interface Check your computer to see which type of serial port is provided then use a connecting cable below 1 Computers with a 25 pin D sub male serial connector should use Connect Cable Labconco part number 7537801 to connect a computer to the Labconco Freeze Dry System 2 Computers with a 9 pin D sub male serial connector should use Connect Cable Labconco part number 7537800 to connect a computer to the Labconco Freeze Dry System The purpose of the RS232 interface is to send data to a data logging computer to monitor the state and activity of the Freeze Dry System This data is half duplex data The data properties are as follows 1 Data Rate 2400 Baud 2 8 Bit word length 3 1 Start bit 1 Sto
118. s 1 4 kg Ampule Valve Adapters 7593401 Adapter connects ampules to valve ports or stainless steel stems Ten per package Shipping weight 0 5 Ib 0 2 kg Stoppers 7572510 Stopper for Stoppering Ampules 75723 10 100 per package Shipping weight 3 Ibs 1 4 kg Trident Adapter 7762700 Three Way Adapter permits attachment of three ampules to a single valve port Ampules are attached using Ampule Valve Adapters or 1 8 surgical tubing not provided Cavity in adapter body can be filled with cotton fiber media to help prevent contamination between samples Shipping weight 3 oz 0 1 kg Product Service Domestic 1 800 522 7658 International 816 333 8811 75 76 DECLARATION OF CONFORMITY Application Council Darective s TYIVEEC 8936 ERC Standard s to which conformity is declared EN61010 EN35022 EN SCHR 2 1 Manufacturer s Mame Labconco Corporation Manufacturer s Address 11 Prospect Avenue Kansas City MO 64132 USA Importer s Name See Shipping Customs Documewis Importer s Address See Shipping Customs Documents for your equipment Type of Equipment Laboratory Equipment Freeze Dryer Model No 775 followed by two digit number based on model size followed by another two digit number based on options 77400 followed by two digit number based on options 79540 followed by two digit number based on options 767 followed by two digit number based om model size followed by anoiber twa digii number base
119. sealing surface of the valve body and reinstall the valve DO NOT APPLY VACUUM GREASE TO THE SAMPLE VALVE GASKETS WHICH SEAL TO THE WALL OF THE DRYING CHAMBER If the valve still seems to be the source of the problem remove the valve and stopper the hole with a rubber stopper Continue checking the other valves Product Service Domestic 1 800 522 7658 International 816 333 8811 43 Chapter 7 Troubleshooting 7 Make sure that the sample valve bulkhead nuts are tight Either tighten by hand or use the wrench supplied with chambers To use the wrench first remove the knob and stem assembly and also the valve body The pins on the wrench fit into the round holes of the nut The nut should be snug but avoid over tightening Replace the valve body knob and stem assembly The illustrations below show how the sample valve installs on a chamber and a manifold Knob amp Stem Valve Body Assembly Valve Assembly Clear Chamber with Valves 44 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 7 Troubleshooting Valve Body Bulkhead Nut Manifold Assembly Knob amp Stem im Ri Assembly Valve Body Trim Ring Knob amp Stem Thrust Washer Gasket Bulkhead Assembly No grease Fittin required 8 Valve Assembly Manifold Valve Assembly Stainless Steel Chamber lll System Components and Collection Chamber Isolation 1 Remove the drying chamber or manifold 2 L
120. ss SELECT until the appropriate offset is shown If the Freeze Dryer is operating on nominal 115V each number represents 2V If 3 is entered into the display the high line alarm will alarm when the voltage raises to approximately 133V for example 127 2x3 133V Ifthe Freeze Dryer is operating on nominal 230V each number represents 4V if 3 is entered into the display the low line alarm will alarm when the voltage drops to approximately 266V for example 254 4x3 266V There will be no alarm indicated if DISABLED is selected Press MENU and the display will show DRYING CHAMBER NOT INSTALLED Press and hold SELECT to change the status Press MENU and the display will show PURGE VALVE NOT INSTALLED Press and hold SELECT to change the status Press MENU and the display will show DEFROST HEATER NOT INSTALLED Press and hold SELECT to change the status Press MENU and the display will show MOISTURE SENSOR INSTALLED Press and hold SELECT if you want to disable the moisture sensor Press MENU and the display again show SHELL FREEZER NOT INSTALLED Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 8 Modifying Your Freeze Dryer Display Press and hold SELECT to change the status Press MENU and the display will show HOLD SELECT TO CLEAR ALL TOTAL HOURS If you want to reset Total Hours press and hold SELECT until an audible beep is heard The display will defa
121. steadily while freeze drying is in progress and turns off if either the programmed cycle is completed or the process is terminated in mid cycle The amber lamp flashes if freeze drying is in progress and an out of specification condition exists Stoppering Controls the stoppering up and down movement The mechanism will function only while the chamber is under vacuum The stoppering action should be closely monitored when operating this control Vacuum Release Vents the chamber so the chamber door can be opened This control can also vent gas into the chamber when the gas is properly connected to the backfill port Back Fill A regulated tank of gas may be connected to the port to allow the introduction of gas into the chamber after freeze drying The port accepts 1 8 tubing Ethylene Oxide is not recommended for use in this Tray Dryer for decontamination because of its hazardous and corrosive properties Power Switch Turns all power to Tray Dryer ON or OFF Not shown Located on left side of cabinet 18 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 4 Using Your Stoppering Tray Dryer Operation Checklist The following checklist should be followed prior to each use of your Stoppering Tray Dryer 1 Wipe out the interior of the Stoppering Tray Dryer chamber with a soft cloth or paper towel to remove any moisture or debris 2 Wipe the interior of the collector chambe
122. stic 1 800 522 7658 International 816 333 8811 59 60 AppeNpIx C FREEZE DRYER SPECIFICATIONS This Appendix contains technical information about the Freeze Dryer including electrical specifications environmental operating conditions and wiring diagrams Electrical Specifications 6L 12L and 18L Console Voltage Amperage w o Max with Catalog Operating Vacuum Vacuum Number Description Nominal Range Frequency Phase Pump Pump 7753020 6 Liter Freeze Dryer 115 103 127 60 1 9 16 100 90 110 50 1 9 16 7753021 6 Liter Freeze Dryer 115 103 127 60 1 9 16 100 90 110 50 1 9 16 7753022 6 Liter Freeze Dryer 115 103 127 60 1 9 16 100 90 110 50 1 9 16 7753024 6 Liter Freeze Dryer 115 103 127 60 1 9 16 100 90 110 50 1 9 16 7753026 6 Liter Freeze Dryer 115 103 127 60 1 9 16 100 90 110 50 1 9 16 7753027 6 Liter Freeze Dryer 115 103 127 60 1 9 16 100 90 110 50 1 9 16 7753030 6 Liter Freeze Dryer 230 198 254 50 1 3 8 7753031 6 Liter Freeze Dryer 230 198 254 50 1 3 8 7753032 6 Liter Freeze Dryer 230 198 254 50 1 3 8 7753034 6 Liter Freeze Dryer 230 198 254 50 1 3 8 7753036 6 Liter Freeze Dryer 230 198 254 50 1 3 8 7753037 6 Liter Freeze Dryer 230 198 254 50 1 3 8 7753040 6 Liter Freeze Dryer 230 187 253 60 1 3 8 7753041 6 Liter Freeze Dryer 230 187 253 60 1 3 8 7753042 6 Liter Freeze Dryer 230 187 253 60 1 3 8 Product Service Domestic 1 800 522 7658 International 816 333 8811 Appendix C Freeze Dryer Specifications Voltage Am
123. substances that are heat sensitive Other than food processing e g coffee whole dinners freeze drying has been extensively used in the development of pharmaceuticals e g antibiotics and preservation of biologicals e g proteins plasma viruses and cell lines The nondestructive nature of this process has been demonstrated by the retention of viability in freeze dried viruses and microorganisms Freeze drying is a process whereby water or other solvent is removed from frozen material by converting the frozen water directly into vapor without the intermediate formation of liquid water The basis for this sublimation process involves the absorption of heat by the frozen sample in order to vaporize the ice the use of a vacuum pump to enhance the removal of water vapor from the surface of the sample the transfer of water vapor to a collector and the removal of heat by the collector in order to condense the water vapor In essence the freeze dry process is a balance between the heat absorbed by the sample to vaporize the Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 1 Introduction ice and the heat removed from the collector to convert the water vapor into ice Freeze Dry Rates The efficiency of the freeze drying process is dependent upon the surface area and the thickness of the sample the collector temperature and vacuum obtained the eutectic point and solute concentration of the sample It is
124. ted above 22 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 4 Using Your Freeze Dryer e Press SELECT until the desired vacuum operating level is displayed See Setting the Operating Vacuum Level for guidelines e 6If 0 is selected the vacuum control is disabled and the vacuum level in the Freeze Dry System will be determined by the capabilities of the vacuum pump e Press MENU e The display will show TEMPERATURE UNITS C F Press SELECT until the desired units are flashing is displayed Press MENU The display will show the following screen if the Freeze Dryer is equipped with a Drying Chamber DRYING CHAMBER SETPOINT XX Y When Y is the units selected above e Press SELECT until the desired temperature is displayed e Press MENU e The display will show REFRIG TOTAL HOUR XXXX SERVICE HOUR XXXX e To reset the SERVICE HOUR to 0 press SELECT This allows you to keep track of the time the refrigeration system operated since it was serviced e The display will show the refrigeration system hours REFRIG TOTAL HOUR XXXX RESET SERVICE HOUR Product Service Domestic 1 800 522 7658 International 816 333 8811 23 Chapter 4 Using Your Freeze Dryer e To reset the service hours to 0 continue to hold SELECT 5 seconds until hours are reset e TOTAL HOUR cannot be reset e Press SELECT e The display will show the vacuum pump ho
125. the Freeze Dryer Deadhead the pump by inserting the vacuum sensor from a secondary vacuum gauge into the end of the vacuum hose and observe the vacuum reading obtained Confirm that the pump is capable of achieving an ultimate vacuum less than 0 010 mBar or approximately 10 microns If an inadequate vacuum reading is obtained the pump has most likely failed and may need to be replaced or rebuilt ll Gaskets Tubing Connections Sample Valves 1 Check all sample valves on the drying chamber manifold and ensure all valves are closed or in the vent position Check to ensure all fittings are tight and sealed properly against the chamber Inspect valves for cracks or cuts Inspect gasket s for cracks or defects Ensure the gasket is clean Apply a thin coat of vacuum grease to the gasket Keep in mind too much vacuum grease can actually cause leaks Check the drain line and ensure the drain plug is installed and the tube appears to be in good condition Check all rubber vacuum tubing for signs of deterioration or cracking Check all connections and make sure they are secure and leak tight When checking the sample valves pull as much vacuum as possible If a vacuum indication is displayed wiggle or rotate the valves and watch the gauge for any fluctuations Fluctuations can indicate a potential vacuum leak If the valve seems to be in good condition remove the valve and apply a thin coat of vacuum grease to the stem and the outside
126. the vacuum pump power cord A plug is supplied that can be installed on the vacuum pump power cord if necessary If the vacuum pump has an off on switch turn the switch on The vacuum pump will be controlled by the Freeze Dryer Connect the vacuum pump inlet port to the vacuum tube inside the cabinet near the front with the vacuum hose and clamps provided If necessary cut the hose to proper length to allow for gentle bends without kinks Vacuum Hose Product Service Domestic 1 800 522 7658 International 816 333 8811 13 Chapter 3 Getting Started 14 The lower front panel is installed by first sliding the top edge under the lip on the plastic control panel Pivot the bottom inward and push until the latch is secure Electrical Connection Plug the power cord into the receptacle on the back of the Freeze Dryer and plug the other end into a suitable power receptacle Drying Chamber or Drying Manifold Installation The drying chamber or drying manifold purchased separately may be positioned directly above the 3 inch port on the top of the Freeze Dryer Follow the instructions supplied with the selected accessory Chemical Resistance of Freeze Dryer Components The FreeZone Freeze Dry System is designed to be chemically resistant to most compounds that are commonly used in freeze drying processes However by necessity the Freeze Dryer is comprised of a number of different materials some of which may be a
127. ts used in the Freeze Dryer may be flammable or hazardous to your health Use extreme caution and keep sources of ignition away from the solvents When using flammable or hazardous solvents the vacuum pump must be vented to a fume hood Hazardous materials such as strong acids or bases radioactive substances and volatile organics must be handled carefully and promptly cleaned up if spilled If a sample is spilled in the collector chamber it must immediately be cleaned up 16 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 3 Getting Started WARNING The disposal of substances used in connection with this equipment may be governed by various Federal State or local regulations All users of this equipment are urged to become familiar with any regulations that apply in the user s area concerning the dumping of waste materials in or upon water land or air and to comply with such regulations Product Service Domestic 1 800 522 7658 International 816 333 8811 17 CHAPTER 4 Usinc Your FREEZE DRYER After your Freeze Dryer has been installed as detailed in Chapter 3 Getting Started you are ready to begin using your Freeze Dryer Read this chapter to learn how to e operate the controls e understand the display e connect samples Do not use the Freeze Dryer in a manner not specified by the manufacturer refer to Appendix C Freeze Dryer Specifications The electrical protection prop
128. ttacked and degraded by certain chemicals The degree of degradation is dependent on the concentration and exposure duration Some of the major components of the FreeZone Freeze Dry System that are susceptible to degradation are as follows Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 3 Getting Started Acids Buffers Solvents z 2 x m o z 5 Sl os E E E E E Q 3 a y 3 a o E g z 3 8 Oo E SE m 3 Ct o E E E gt v lt 3 5 E E v a o z o 2 5 E E ES amp B amp B S E E E 3 3 a amp E 5 Component Material moa E oe ou E e Valve Stem Acetal C DD D D Delrin Collector Acrylic D D D Lid Hoses Neoprene C DD Cc C D D C D Gaskets amp Valve Bodies Flask Top Silicon C D D D D D C D Rubber Chamber amp Stainless C Fittings Steel An accessory glass lid is available C D Moderate degradation Limited use Severe degradation infrequent use recommended immediate thorough cleaning required Most common compounds used in freeze drying processes if allowed to enter the vacuum pump will degrade the oil and cause damage to the vacuum pump Sugars and proteins typically will have minimal negative effect on any of the materials of construction When using compounds in the Freeze Dryer that are hostile to the materials of construction it is imperative the equipment is thoroughly cleaned after use Product Service
129. ube to the exposed port service port The port is 3 8 x 45 male flare Item 4 5 Remove the fluid reservoir cover Item 2 and place the opposite end of the tubing into the fluid reservoir Product Service Domestic 1 800 522 7658 International 816 333 8811 47 Chapter 7 Troubleshooting 6 7 8 9 10 11 12 13 Fill the reservoir slowly allowing the fluid to drain through the system When the system appears full prepare to start the circulation pump Open the fluid circulation valve by completely down seating turn top valve stem completely clockwise to direct fluid to by pass through tubing to fluid reservoir Attach the power wires to the power switch Activate the pump by moving the Power switch to the ON position The control panel does not need to be installed If it is installed the RUN STOP switch must be off The fluid system will circulate with the fluid going through the add on tubing purging itself of air Add fluid when needed to keep fluid in the reservoir After the fluid stream is established tilt the stoppering system up and down Observe the fluid stream and repeat the tilt procedure if it is not free of bubbles After the system is free of air up seat fluid circulation valve turn valve stem completely counter clockwise closing the fluid tubing by pass Set the controller to operate at 24 C 75 F in the manual mode Push the Run Stop
130. ult to the main freeze dry display information If you do not want to set Total Hours press MENU and the display will show PRODUCTION MENU MASTER RESET The routine will repeat by pressing MENU or want approximately 10 seconds for the display to default to the main freeze dry information display information In order to store offsets in memory you Must Press and Hold MENU until the display shows PASSWORD Wait approximately 10 seconds and the display will default to the main freeze dry display information This can be done anytime throughout the Modifying the Display routine Product Service Domestic 1 800 522 7658 International 816 333 8811 53 APPENDIX A FREEZE DRYER COMPONENTS The following pages list components that are available for your Freeze Dryer The parts shown are the most common replacement parts If other parts are required contact Product Service ED DDT TT TODOS a se 54 Product Service Domestic 1 800 522 7658 International 816 333 8811 Appendix A Freeze Dryer Components Item Model Part No Description l All 7689900 Lid Gasket Collector 2 All 7532900 Lid Collector 3 All 7408400 Lid Gasket Drying Chamber Shell Freezer 4 All 7408300 Lid Drying Chamber 6L 7403100 Lid Shell Freezer 5 6L 7750602 Compressor 115V 60 Hz
131. ure of the sample Product Service Domestic 1 800 522 7658 International 816 333 8811 27 Chapter 4 Using Your Freeze Dryer Adding Sample The following procedure should be followed when using sample valves in the freeze dry process 1 Connect a pre frozen sample to a sample valve on the drying chamber or manifold using an adapter Turn the plastic valve knob to the VACUUM position to open the valve The bevel on the knob should be positioned toward the sample port to apply vacuum to the sample Bevel in vent position Vent Backfill Port Bevel in vacuum iy position Adapter 2 Before adding another sample allow system vacuum to return to 0 133 mBar or lower Any combination of valves and sample sizes may be utilized at one time provided that the system vacuum and collector temperature remain sufficiently low to prevent melting of the frozen sample When all the frost has disappeared from the outer surface of the sample container and no cold spots can be detected by handling the container the sample is nearly dry To be certain of low final moisture content dry the sample for several hours past this point To remove a container after drying is complete turn the plastic knob on the valve to the VENT position which closes the valve and vents the container Should backfilling with an inert gas be required connect the gas supply line to the vent port on the valve before turning the
132. urs VACUUM TOTAL HOUR XXXX SERVICE HOUR XXXX e To reset the SERVICE HOUR to 0 press SELECT e The display will show VACUUM TOTAL HOUR XXXX RESET SERVICE HOUR If you want to reset the service hours to 0 continue to hold SELECT five seconds until hours are reset e Press SELECT e The display will show the RS 232 data transmission rate RS 232 TRANSMISSION RATE 10 SECONDS e To change the rate press and hold SELECT until the desired time interval is shown The time between data transmissions may be set to occur at 10 30 60 300 or 600 second intervals e Press SELECT to return to display operating parameters or after a short delay the display will automatically switch to show operating parameters 24 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 4 Using Your Freeze Dryer Baffle 6 Liter 84 C Cascade model 12 Liter 84 Cascade model amp 18 Liter Model Position the baffle so it rests on the top of the collector coil The arrow should point toward the front Automatic Start Up Models not equipped with a purge valve To run the Auto Mode press the panel switch labeled REFRIGERATION AUTO The green LED above the switch will illuminate This will start the refrigeration system When the collector reaches 40 C the vacuum pump will start The Temperature and Vacuum Graphs will indicate collector temperature and system vacuum The LCD display will show
133. ween MIN and MAX If the oil level is less than an inch 25 4 mm above MIN add oil to proper level Product Service Domestic 1 800 522 7658 Chapter 5 Maintaining Your Stoppering Tray Dryer 5 If oil shows cloudiness particles or discoloration drain the pump and replace with fresh oil 6 Utilization of acids requires immediate cleaning and neutralization after a run or physical damage will result Monthly 1 The rubber components on the Stoppering Tray Dryer may eventually deteriorate and require replacement The effective life of rubber parts depends upon both their usage and the surrounding environment Check all rubber hoses and gaskets and replace any that show signs of hardening permanent set or deterioration 2 Using a soft cloth sponge or chamois and a mild non abrasive soap or detergent clean the acrylic door 3 Using a soft cloth sponge or chamois and a mild non abrasive soap or detergent clean the exterior surfaces of the unit Liquid spray cleaners and polishes may be used on the exterior surfaces Do not use solvents to remove stains from the exterior surfaces as they may damage the finish Annually 1 Every 12 months or more often if the Stoppering Tray Dryer is operated in a dusty environment the refrigeration system condenser should be cleaned Using a vacuum cleaner with brush attachment clean the condenser to ensure proper airflow for peak performance Decontamination When freeze d
134. y 7390702 Baffle 6L Cascade only 7390701 Baffle 12L Cascade only 7390700 Baffle 18L Only 12 If you did not receive one or more of the components listed for your Freeze Dryer or if any of the components are damaged contact Labconco Corporation immediately for further instructions Setting Up Your Freeze Dryer After you verify receipt of the proper components move your Freeze Dryer to the location where you want to install it Then follow the steps listed below Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 3 Getting Started Vacuum Pump Connection A vacuum pump as described in Chapter 2 Prerequisites is required to operate your Freeze Dry System properly The Freeze Dryer is equipped with a 3 4 ID heavy wall vacuum hose for connecting the collector chamber to the vacuum pump Make certain that the oil in the vacuum pump is at the proper level Remove the front stainless steel panel or lower rear panel from the Freeze Dryer The front panel is removed by placing a flat blade screw driver into the rectangular hole in the center of the kick panel Pivot the handle downward to disengage the latch and simultaneously pull the lower panel forward Place the vacuum pump inside the cabinet Connect the vacuum pump power cord to the receptacle on the back of the cabinet labeled vacuum pump Models rated for use on 230V have a reverse IEC connector for attaching
135. ycles have been programmed push the MODE button to Select AUTO Push the RUN STOP button to start the program running The RUN indicator will light The System 24 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 4 Using Your Stoppering Tray Dryer Status Display will change and the Display will change to MONITOR mode During the RAMP cycle of the active segment the Status Display will be as follows Pl Pl PRB 1 28 2 29 3 28 C indicates what program is selected shelf probes for shelf 1 2 and 3 If a probe is not installed the display shows C F system temperature indicates what segment is active and ramping system vacuum level mBar Pascal Torr During the HOLD cycle of the active segment the Status Display will alternately be as follows Pl PRB1 28 2 29 3 28 C n TMP 30 SEG 1H VAC 030 M PBR TMP SEG VAC P1 PRB1 28 2 29 3 28 C TR TMP 30 TR 4 55 VAC 0033 M indicates what program is selected shelf probes for shelf 1 2 and 3 system temperature indicates what segment is active and holding system vacuum level indicates the amount of time remaining in the present seg ment If time is 10 0 hours or more the time is displayed in 1 10 hours If time is less than 10 0 hours the time is displayed in 1 100 hours If the hold time was programmed to be indefinite the display will show INDF Product Service Domestic 1 80
136. yer 230 50 x x 7753036 6 Liter Freeze Dryer 230 50 x x 7753037 6 Liter Freeze Dryer 230 50 x x x 7753040 6 Liter Freeze Dryer 230 60 7753041 6 Liter Freeze Dryer 230 60 x 7753042 6 Liter Freeze Dryer 230 60 x 7753044 6 Liter Freeze Dryer 230 60 x x 7753046 6 Liter Freeze Dryer 230 60 x x 7753047 6 Liter Freeze Dryer 230 60 x x 7753522 6 Liter Freeze Dryer 115 60 x x 7753524 6 Liter Freeze Dryer 115 60 x x x 7753532 6 Liter Freeze Dryer 230 50 x x 7753534 6 Liter Freeze Dryer 230 50 x x x 7753542 6 Liter Freeze Dryer 230 60 x x 7753544 6 Liter Freeze Dryer 230 60 x x x 10 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 3 Getting Started Catalog Numbers 6 12 and 18 Liter Console Models Teflon Catalog Coated Purge Drying Shell Number Description Volts Hz Chamber Valve Chamber Freezer 7934020 6 Liter Cascade Freeze Dryer 115 60 7934021 6 Liter Cascade Freeze Dryer 115 60 x 7934022 6 Liter Cascade Freeze Dryer 115 60 x 7934024 6 Liter Cascade Freeze Dryer 115 60 x x 7934026 6 Liter Cascade Freeze Dryer 115 60 x x 7934027 6 Liter Cascade Freeze Dryer 115 60 x x x 7934030 6 Liter Cascade Freeze Dryer 230 50 7934031 6 Liter Cascade Freeze Dryer 230 50 x 7934032 6 Liter Cascade Freeze Dryer 230 50 x 79
137. yer Accessories for the baffle part number See the section titled Baffle in this chapter for proper installation Some guidelines for setting the Freeze Dryer are shown below These show pre freezing temperatures and vacuum levels Exact protocols must be determined by the user for the specific samples that are being freeze dried Material Solidification Eutectic Pre Freeze Vacit Set Point Temperature Temperatures Bacteria Virus 40 C and Colder 50 C amp 0 040 mBar amp Colder Lower Milk 5 to 13 15 to 23 1 65 to 0 77 Fungi 40 and Colder 50 amp Colder 0 04 and lower Vegetable Tissue 25 to 50 35 to 60 0 22 to 0 01 Human Tissue 30 to 40 40 to 50 0 12 to 0 04 Blood Plasma 10 to 25 20 to 35 1 03 to 0 22 Vaccine 30 to 40 40 to 50 0 12 to 0 04 Pre Freezing Samples Appropriate containers for freeze drying include ampules serum bottles and wide mouth freeze drying flasks Shell freezing of samples is recommended for wide mouth freeze drying flasks Smaller samples in ampules and serum bottles may be frozen in a freezer The sample container size should always be at least two to three times the sample size i e 40 ml samples should be prepared in 80 ml containers or larger The temperature required for pre freezing is dependent on the characteristics of the sample Pre freezing temperature typically is at least 10 to 20 C below the eutectic or collapse temperat

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